Journal of Environmental Chemical Engineering 9 (2021) 105731

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Journal of Environmental Chemical Engineering

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

Reuse of water from real reactive monochromic and trichromic wastewater

for new cotton dyes after efficient treatment using H2O2 catalyzed by
UV light
Katia Crystina Hipólito Bezerra a, 1, Ticiane Rossi Fiaschitello b, 2, Geórgia Labuto c, *, 3,
Harold S. Freeman d, 4, Wallace Duarte Fragoso e, 5, Sirlene Maria da Costa b, *, 6,
Silgia Aparecida da Costa b, 7
a
Faculdade de Tecnologia Antoine Skaf, Rua Correia de Andrade, 232 - Brás, 03008-020 São Paulo - SP, Brazil
b
School of Arts, Sciences and Humanities, Textile and Fashion Course, University of São Paulo, Av. Arlindo Béttio, 1000, Parque Ecológico do Tietê, Ermelino
Matarazzo, 03828-080 São Paulo, SP, Brazil
c
Laboratory of Integrated Sciences, Department of Chemistry, Universidade Federal de São Paulo, Rua. Prof. Artur Riedel, n◦ 275, 09972-270 Diadema, SP, Brazil
d
College of Textiles, North Carolina State University, 1020 Main Campus Drive, Raleigh, NC 27695-8301, United States
e
Universidade Federal da Paraíba, Centro de Ciências Exatas e da Natureza - Campus I, Departamento de Química. Cidade Universitária, 58059-900 João Pessoa, PB,
Brazil

A R T I C L E I N F O A B S T R A C T

Editor: Dr. GL Dotto The textile industry widely uses reactive dyes to obtain cotton fabrics having good resistance to color removal
despite frequent washing. This level of dye usage generates substantial volumes of wastewater containing sig­
Keywords: nificant quantities of residual dye requiring treatment before discharges from commercial dyeing operations to
Cycles of reuse public waterways. As part of a study aimed at recycling/reusing rather than discharging reactive dye wastewater,
Wastewater
well-known dyes Reactive Yellow 176, Reactive Red 241, and Reactive Blue 221 were used in dyeing cotton
Reactive dyes
fabric, and the generated wastewater samples were decolorized with H2O2 catalyzed by UV light. The efficiency
Trichromy
UV light of UV/H2O2 decolorization for trichromic wastewater was determined by UV-Vis monitoring at 550 nm, wherein
Hydrogen peroxide it was found that more than 91% of color removal in trichromic wastewater occurred at pH 4. The reuse of
wastewater was investigated by a total of three sequential cycles of wastewater treatments. The quality of cotton
dyed with reused wastewater was assessed through color measurements using CIELAB, fastness to light, and wash
fastness testing. Results showed that MCT/VS-based reactive dye wastewater arising from UV/ H2O2 treatment
could be used for two subsequent dyeing cycles without compromising the quality of the color of the dyed cotton
fabrics. The proposed treatment can also save water and salt, enhancing the economy of the dyeing process.

1. Introduction achieve this goal is responsible for water use by optimizing and
reviewing industrial processes that minimize its uses and contamination
Water security is one of the Sustainable Development Goals estab­ and allow its reuse. In contrast, the textile industry is one of the most
lished by the United Nations (UN, 2015). Among the actions necessary to polluting industries in the world [1–3] due to the generation of large

* Corresponding authors.
E-mail addresses: katia.bezerra@unifesp.br (K.C.H. Bezerra), ticianerossi@gmail.com (T.R. Fiaschitello), geolabuto@gmail.com, georgia.labuto@unifesp.br
(G. Labuto), hfreeman@ncsu.edu (H.S. Freeman), wallace@quimica.ufpb.br (W.D. Fragoso), sirlene@usp.br (S.M. da Costa), silgia@usp.br (S.A. da Costa).
1
https://orcid.org/0000-0001-8034-9517
2
https://orcid.org/0000-0002-4668-7640
3
https://orcid.org/0000–0002-5403–8974
4
https://orcid.org/0000–0002-9578–7250
5
https://orcid.org/0000–0003-2546–7769
6
https://orcid.org/0000–0003-0522–0611
7
https://orcid.org/0000–0001-8331–538X

https://doi.org/10.1016/j.jece.2021.105731
Received 18 March 2021; Received in revised form 10 May 2021; Accepted 22 May 2021
Available online 25 May 2021
2213-3437/© 2021 Elsevier Ltd. All rights reserved.
K.C.H. Bezerra et al.
volumes of effluent containing residual (unexhausted) dyes and chem­
ical auxiliaries used in dyeing processes [4]. The average water con­
sumption for dyeing with synthetic dyes ranges from 30 to 50 L/kg of
fabric and about 60 L/kg of yarn depending on the process, the fiber, and
the dye to be used [5–7]. The estimated annual production of synthetic
dyes is 7 × 105 tons, and 10–50% of this dye remains in the associated
effluent that needs to be treated before release into the environment [8].
This is because textile dyes in natural water bodies can increase
turbidity, interfering with sunlight’s penetration, which causes a
reduction in the algal photosynthesis rate for various aquatic plants.
Consequently, this reduces the concentration of oxygen in the water,
damaging water quality, causing toxic effects, and hindering the process
of self-purification [9,10].
Reactive dyes are the most extensively used colorants in the textile
industry due to their ability to give a wide range of wash-resistant shades
on cotton through covalent bond formation [11]. The high consumption
of these dyes for dyeing cotton gives rise to environmental concerns
since a significant amount of the dyes remains with the effluent due to a
competing dye hydrolysis reaction during the dyeing process, which can
lead to dye–fiber fixation levels at low as 50% [12]. Fig. 1A illustrates
the competing reactions when dyeing cotton fibers with a reactive dye:
dye fiber fixation (1) and dye hydrolysis (2). Dye hydrolysis produces a
Fig. 1. A) Competing reactions when dyeing cotton fibers with a reactive dye: dye–fiber fixation (1) and dye hydrolysis (2), and B) examples of bireactive dyes for
enhanced dye–fiber fixation.
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Journal of Environmental Chemical Engineering 9 (2021) 105731
product (2) that cannot form a covalent bond to the cotton, giving a
highly colored effluent. To enhance dye–fiber fixation levels, dyes
containing two or more reactive groups are used. Thus, a monoreactive
dye giving 80% fixation could give up to 96% fixation upon conversion
to a bireactive dye with two chances to bond to the fiber. The initial
homo/hetero-bireactive dyes were of types 3 and 4 (Fig. 1B), but the
heterobireactive dyes containing MCT-VS (e.g. 4) and MFT-VS (mono­
fluortriazine vinyl sulfone) systems have come to the forefront.
Currently, in addition to the interest in reducing the consumption of
water and chemicals in textile processes, there is a search for technol­
ogies to remove color and technologies that can produce reusable water,
remove toxicity, mineralize aromatic compounds, or recover unbound
dyes [2,13]. Different methods for decolorizing textile industry effluents
have been used since there is no perfect one to solve all questions. In this
regard, physical (membrane flotation, adsorption), electrochemical
(oxidation/reduction), chemical (e.g. ozonation/chlorination), and
biological (e.g. anaerobic/aerobic) techniques have been applied to
anionic, nonionic, and cationic dyes to give high color removal [14,15].
Similarly, updates about the use of electrocoagulation [8] and
membrane-based techniques [16] in textile effluent treatment have been
published. In the former review, electrocoagulation was reported to be
of interest due to its versatility and environmental compatibility and
K.C.H. Bezerra et al.
faster speed than chemical coagulation. Studies about anionic, nonionic,
and cationic dyes were cited, including dye mixtures.
Concerning chemical treatments, one of the methods that have
received a great deal of attention for textile effluent treatment is the
advanced oxidation process (AOP) [17,18]. This technology’s funda­
mental goal is to improve the wastewater’s quality before disposal or
reuse by mineralization of dye molecules. Using an AOP, complex sub­
stances in dye wastewater are oxidized by hydroxyl radical formation
and use [19]. Hydroxyl radicals have an oxidation potential that is
second only to fluorine radicals and are generated mainly using UV,
UV/O3, and UV/H2O2 systems [20]. UV/H2O2 systems have been
applied to the degradation of various pollutants [21,22]. Advantages to
their use include: 1) H2O2 can be readily mixed with water in all pro­
portions; 2) costs associated with a UV/H2O2 system are smaller than
those associated with related processes such as UV/O3; 3) UV/H2O2
treatments lead, in most cases, to the mineralization of organic pollut­
ants, and 4) a sludge does not form after the treatment [23]. Addition­
ally, visible light can also be used for photocatalytic degradation of a
Fig. 2. Structures in the MCT/VS reactive dye combination used in the present study, C.I. Reactive Yellow 176 (YELLOW), C.I. Reactive Red 241 (RED), and C.I.
Reactive Blue 221 (BLUE).
3
Journal of Environmental Chemical Engineering 9 (2021) 105731
textile dye in the presence of carbon-doped TiO2, taking advantage of
the fluorescence properties of dyes such as Rhodamine B [24].
Considering the large volumes of commercially reactive dyes used,
studies involving removing textile wastewater [25–28] and the reuse of
reactive dye wastewater [2] have been reported. However, most previ­
ous studies used synthetic wastewater [28], and little is published about
using AOP to treat dye wastewater containing a trichromic combination
of reactive dyes and reuse of the treated water in a subsequent dyeing
process [29]. In the present study, three widely used azo and formazan
MCT-VS bireactive dyes, C.I. Reactive Yellow 176 (YELLOW), C.I.
Reactive Red 241 (RED), and C.I. Reactive Blue 221(BLUE), were used
separately and in combination to dye cotton fabric. These dyes were
chosen since various combinations produce a range of colors frequently
used in the textile industry, and their molecular structures are known.
The generated wastewater samples were treated with UV/H2O2 and used
to dye new cotton fabrics with the same dyes, achieving three sequential
cycles of dyeing-effluent treatment-wastewater reuse. To confirm the
viability of the proposed treatment to allow the reuse of water in new
K.C.H. Bezerra et al.
dyeing, ensuring the viability of the process, coloristic and fastness
properties of the dyed fabrics were compared using the initial and
treated water.
2. Material and methods
This research was conducted mainly in the Laboratory of Chemistry
in the School of Arts, Sciences and Humanity, at the University of São
Paulo, with fastness analysis conducted in the School SENAI Francisco
Matarazzo.
2.1. Dyes
The dyes, C.I. Reactive Yellow 176 (YELLOW), C.I. Reactive Red 241
(RED), and C.I. Reactive Blue 221 (BLUE), and organic auxiliary com­
pounds used in this study were obtained from commercial sources in
Brazil and were used as received. Inorganic dyeing auxiliaries were
obtained from Sigma-Aldrich Company. The catalase enzyme (Goldzima
HPX) was kindly provided by Golden Technology do Brazil, enzymatic
activity (≥ 19,000.0 CIU/mL). Fig. 2 presents the structural formula for
the reactive dyes involved in the present study.
2.2. Dyeing process for wastewater production
The first fabric dyeing was conducted with tap water, using 5 g
samples of 100% bleached cotton fabrics and a liquor ratio of 1:10 and a
Mathis machine model ALT-B dyeing machine. The fabric was added to a
monochromic (1.10% of individual YELLOW, RED or BLUE dye) or tri­
chromic (0.4% YELLOW, 0.4% RED, 0.4% BLUE) dyebath consisting of
1 g/L sequestering agent and 65 g/L NaCl at room temperature. The
bath temperature was raised to 60 ºC over the next 15 min, and sufficient
alkali was added to give a bath concentration of 1.5 g/L NaOH, 5 g/L
Na2CO3, and the temperature was held for 30 min. Acetic acid (2 mL/L)
was added, and dyeing was continued for 1 h. The bath was dropped and
replaced by 1 g/L anionic detergent, and the fabric was washed for
5 min at 50 ºC, then given two 15 min washes in 1 g/L detergent at 90 ºC,
followed by a 5 min water rinse at 50 ºC, and dried.
All wastewater generated from the dyeing and washing steps was
collected and used in the UV/H2O2 treatment step.
Fabrics dyeing using decolorized wastewater was conducted ac­
cording to the procedure described above. The only difference was
substituting the tap water with wastewater from the UV/H2O2 treat­
ment. The amounts of reagents were the same, except for the quantity of
NaCl used, which was adjusted according to the treated wastewater’s
conductivity, calculated from a calibration curve, as described in item
2.4.3.
2.3. Wastewater treatment with UV/H2O2
2.3.1. Effect of pH on wastewater on color removal by UV/H2O2
Wastewater samples obtained from the monochrome and trichrome
dye baths and cotton fabrics washings were divided into three 500 mL
samples. The pH was adjusted to 4.0, 7.0, and 11.0, respectively, using
4 mol/L acetic acid or 4 mol/L NaOH, as needed. To each sample was
added 14.7 mmol/L of H2O2 (50% v/v). The wastewater samples were
placed in an Osram photochemical reactor covered with aluminum foil
to avoid the loss of emission rays and equipped with three 254 nm UV
lamps of 1.7 watts each, having an average lifetime of about 8000 h. The
UV lamps were positioned on the top of the reactor at 10 cm from the top
of the wastewater vessels. The loading and removal of wastewater were
performed by a door equipped with a glass filter for UV, which
remaining closed during the wastewater assays. The reactor was also
equipped with a cooler to refresh the system and maintain the
4
Journal of Environmental Chemical Engineering 9 (2021) 105731
temperature, monitored by a thermocouple inserted through a hole in
the reactor wall and reaching the wastewater under treatment. The
temperature was maintained at 25 ºC during all wastewater treatments.
Each wastewater sample was positioned on a magnetic stirrer to main­
tain constant agitation during the treatment (200 rpm). Samples were
collected for analysis at 00, 20, 40, 60, 90, 120, 150, 180, 210, 240, 270,
300, and 330 min of irradiation employing a syringe connected to
wastewater vessels by a little hose placed inside the solutions so as not to
interrupt the treatment. The UV/H2O2 treatment was conducted over
5 h. Fig. S1 (Supplementary Data) presents a scheme of the reactor.
At the end of UV/H2O2 treatment, 0.2 mL/L catalase (Goldzima
HPX) was added to decolored wastewater to eliminate all residual H2O2
that could interfere in new dyeings employing the treated wastewater.
The efficiency of color removing by UV/H2O2 treatment was monitored
by a colorimetric method using a Beckman DU 640 UV–visible spec­
trophotometer over the 280–700 nm region (λmax: YELLOW = 412,
RED = 528, BLUE = 592 and Trichromic effluent = 550 nm, the spectra
of wastewater are available as Supplementary Data, Fig. S2). The
percent color removed was calculated using Eq. (1),
Ai-Af
Color removed (%) = × 100 (1)
Ai
Where:Ai = initial absorbanceAf = final absorbance.
The water from samples treated by UV/H2O2 was reserved for new
dyeing of cotton fabrics employing the same monochromic and tri­
chromic baths and with the same dyeing procedure. Control experiments
using the same pH values, times, and H2O2 additions in dark experi­
ments (without UV irradiation) did not promote dye degradation, which
is in accordance with the literature because HO• species are not
produced.
2.4. Viability of reuse water from samples treated by UV/H2O2
2.4.1. Evaluation of TOC in dye wastewater before and after UV/H2O2
treatment
The total organic carbon (TOC) analysis in water from samples
treated with UV/H2O2 was conducted to determine the level of miner­
alization, an indicator of the UV/H2O2 treatment [30]. Total organic
carbon (TOC) levels of the samples obtained from the photochemical
treatment were determined in collaboration with the Laboratory of
Engineering and Environmental Control of Unifesp, Diadema, and São
Paulo. Wastewater samples obtained after the UV/H2O2 treatment were
acidified with HNO3 (1 mol/L), separated into 3.0 mL aliquots, filtered
through 0.45 µm filters diluted to 30 mL with distilled deionized water.
The samples were then subjected to quantification of total organic car­
bon (TOC).
2.4.2. Color levels in trichromic wastewater before and after UV/H2O2
treatment
The color levels of dyes in trichromic wastewater and reused water
obtained from their treatments by UV/H2O2 were monitored by UV-Vis
employing a colorimetric method using a Beckman DU 640 UV–visible
spectrophotometer over the 280–700 nm region. This monitoring was
conducted to evaluate the efficiency of UV/H2O2 on removing the color
of the wastewater and prevent the presence of residues of hydrolyzed
dyes since they could interfere with fabric color quality in a subsequent
dyeing cycle. The most intense wavelength observed for the studied dyes
(550 nm) was used to monitor color removal.
2.4.3. Correction of conductivity in dye wastewater reused after UV/H2O2
treatment
Since wastewater produced with reactive dyes tends to have high
conductivity values due to the high concentrations of electrolytes, which
K.C.H. Bezerra et al.
are essential to the dyeing process [31], conductivity monitoring was
carried out to assess the need for its correction. Knowing the conduc­
tivity value of reused water is necessary to enable the use of the elec­
trolyte present in the water from the treated wastewater, saving inputs
from the dyeing cycles.
Although other ionic components are present in the textile effluent,
NaCl contribution to the conductivity is preponderant, both due to its
high concentrations in the dyeing process and its high ionization degree.
For these reasons, NaCl was used to monitor and correct wastewater
conductivity before and after treatment. Thus, for the conductivity
measurement, an analytical curve (equation y = 1718∙x, and R2 =
0.996) was constructed with different NaCl concentrations (0.1–1.2 g/
L), which was used to monitor the conductivity of the water from the
sample treatments. From the conductivity values, corrections were made
to the NaCl concentration in the water to adjust it for reuse in new
dyeing cycles.
2.5. Assessment of cotton dyed with reused water from wastewater treated
with UV/H2O2
The assessment of the viability of employment of the monochromic
and trichromic wastewater samples treated with UV/H2O2 was per­
formed by monitoring the quality of cotton fabric dyed with reuse water.
The quality was evaluated by monitoring the coloristic properties and
fastness testing of the fabrics.
2.5.1. Coloristic properties
After the dyeing with tap water and wastewater treated by UV/H2O2,
cotton fabric samples were compared by colorimetric analysis using a
Konica Minolta spectrophotometer. The L*, a*, b* and ∆E * values were
measured over the 360–700 nm region, using CIE illuminant D65, and
an observer angle of 10º. L* is a measure of the lightness/darkness of the
fabric, which ranges from 100 (white) to 0 (black); a* is a measure of the
redness/greenness of the fabric, with positive values indicating red and
negative values green; and b* is a measure of the yellowness/blueness of
the fabric, with positive values yellow indicating and negative values
blue. The greater the magnitude of a* and b* values, the deeper the
colors.
2.5.2. Fastness testing
Colorfastness to light and washing was also performed on the dyed
cotton samples. The colorfastness to washing was determined according
to ISO (2005a) [32]. The difference between the control fabric and the
Fig. 3. Influence of pH on color removal for monochromic and trichromic wastewater employing samples treated with UV/H2O2. Treatment conditions: 14.7 mmol/
L of H2O2, total time: 5 h, n = 3. UV-Vis monitoring wavelength: YELLOW = 412 nm, RED = 528 nm, BLUE = 592 nm and Trichromic wastewater = 550 nm.
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Journal of Environmental Chemical Engineering 9 (2021) 105731
multi-fiber, before and after washing, was visually compared with the
grayscale to obtain the color change and the staining ratings, according
to the ISO (2005a) and ISO (2005b) [32,33]. The rating scale is 1 (poor)
to 5 (excellent). The lightfastness of dyed fabrics was determined ac­
cording to the AATCC (2014a) [34]. Light exposures were conducted at
an irradiance level of 55 Wm-2, relative humidity of 50%, a black body
temperature of 63 ºC, and chamber temperature of 30 ºC at 5, 10, and
20 h. The differences obtained between the control fabric and the
exposed fabrics were visually assessed using the grayscale to get the
color change values, according to the AATCC (2014b) [35]. The rating
scale is 1 (poor) to 5 (excellent).
3. Results and discussion
3.1. Wastewater treatment with UV/H2O2
3.1.1. Effect of pH on wastewater color removal by UV/H2O2
After dyeing, the wastewater pH is around 11 and, after neutraliza­
tion, is about 7. It would be good if the wastewater could be efficiently
treated at these pH levels without reagents to adjust the pH to acidic
conditions. However, it is known that the degradation of dyes using
H2O2 catalyzed by UV light is more effective under acidic conditions
[36,37]. The organic matter oxidation promoted by UV/H2O2 occurs by
hydrogen abstraction, electron transfer, and radical addition [38].
Among the factors that affect H2O2 photolysis, pH is one of the most
relevant, being the rate of the degradation rate of organic matter
strongly dependent on the acidity of the reaction medium [39,40]. At
basic pH, H2O2 is deprotonated, generating an equilibrium between
H2O2/HO-2 [41]. The coexistence of these two species leads to the re­
action of the H2O2 molecule not dissociated with the HO-2 species,
forming oxygen and water by-products instead of the desired hydroxyl
radical, described in reaction 1 [42]. A decomposition H2O2 reduces the
availability of HO• available in the reactional medium, affecting the rate
of degradation. In addition, H2O2 exhibits higher self-decomposition in
basic pH, also HO• formation [42,43].
HO−2 ⋅ + H2 O2 →H2 O + O2 ⋅ + OH− (Reaction 1)
It is necessary to use acids as reagents to reach acid pH, increasing
the cost of treatments. Thus, three pH levels were investigated for
wastewater treatments. The pH 4 level was chosen instead of a lower
one, precisely as a criterion for saving reagents needed to adjust the pH.
Fig. 3 shows the color removal (%) for monochromic and trichromic
wastewater treated by UV/H2O2 at different pH values. Color removal
K.C.H. Bezerra et al. Journal of Environmental Chemical Engineering 9 (2021) 105731

levels were calculated by comparing treated and the untreated effluent, 2 HO2 ⋅→O2 + H2 O2 (Reaction 7)
using Eq. 1 and absorption maximum of 550 nm. The results indicate
that acidic media facilitates the decolorization treatment. In this study, R − H + HO⋅→R⋅ + H2 O (Reaction 8)
no direct correlation between pH and color removal levels was observed
for all wastewater treatments. For wastewater containing YELLOW and The degradation process of organic matter proceeds in two main
trichromic dye, the order of pH for decolorization efficiency was in steps, firstly the HO• is produced by direct H2O2 photolysis by UV
accordance with the expected (pH 4 > pH 11 > pH 7). The efficiency of irradiation, which is followed by the oxidation of organic compounds by
decolorization for BLUE effluent was very similar for pH 7 and 11. In these radicals [44]. As an advantage, the H2O2 is easily converted to
contrast, for RED wastewater, pH 11 was more efficient than 7, indi­ harmless oxygen and water, and it is a cost-effective reagent. The
cating that color loss was more significant under acidic and alkaline presence of HO• accelerates the degradation process, saving energy by
conditions than under neutral conditions. It is important to note that for reducing the time for degradation and promoting a more efficient
trichromic dye wastewater, pH 4 and 7 showed removal efficiency of mineral assessment of organic compounds, including polycyclic and
around 91%, suggesting that it is possible to treat the wastewater at the aromatics. It is important to mention that despite the rate of
lowest cost.
It is known that bleaching cotton with H2O2 under alkaline condi­
tions generates per hydroxyl ions (HO-2) as the active species, promoting
the degradation of organic substances and possibly degrading dyes [37].
On the other hand, forming this agent reduces hydroxyl radicals (HO•),
which are more reactive species, thus decreasing decolorization
efficiency.
The photochemical oxidation of H2O2 by UV light produces HO•,
capable of degrading organic matter [44]. The mechanism of HO•
degradation of organic matter at decreasing pH is not entirely certain.
However, the following equations are presented in the literature [44,
45]:

(Reaction 2)
hν
H2 O2 → 2HO⋅

H2 O2 + HO⋅→HO2 ⋅ + H2 O (Reaction 3)
Fig. 5. Elimination of color in trichromic wastewater before and after UV/H2O2
H2 O2 + HO2 ⋅→O2 + H2 O (Reaction 4) treatment and successive dyeing/treatment cycles. Treatment conditions:
14.7 mmol/L of H2O2 50% v/v, total time: 5 h, pH treatment = 4, n = 3. UV-Vis
2 HO⋅→H2 O2 (Reaction 5) monitoring wavelength: 550 nm.

HO⋅ + HO2 ⋅→O2 + H2 O (Reaction 6)

Fig. 4. Projected initial UV/H2O2 decolorization products of MCT-VS red dye.

6
K.C.H. Bezerra et al.
disappearance of the HO•, increase in a medium rich in Cl- as the dyeing
wastewater, by producing of HOCl-•, previous studies concluded that
the influence of Cl- upon the photodecomposition of HO• is negligible
[45].
The combination of UV light and H2O2 irreversibly destroyed the dye
chromophore. The reactions are driven by HO• during UV/H2O2
oxidation, and UV photocatalysis of organic pollutants promotes hy­
droxylation, dealkylation, decarboxylation, and deamination, the last
two of which occur even for chains or aromatic rings [46]. For the RED
dye, HO• attack at the hydrazone moiety could lead to the formation of
degradation products of the types shown in Fig. 4, which undergo a
further transformation [47]. For instance, the electrophilic diazonium
compound (5) is subject to hydrolysis, which would give the corre­
sponding desulfonated naphthol. It eliminates the re-coupling potential
of a diazonium intermediate.
Similarly, the intermediate naphthoquinone (6) is subject to further
HO• attack, including the unraveling of the quinone ring. The mecha­
nism of decolorization of the dyes involved in the present work probably
is similar to this one. The presence of H2O2 in dark experiments does not
promote dye degradation, which is in accordance with the literature
because the HO• is not produced.
3.2. Viability of reused dye wastewater treated with UV/H2O2
3.2.1. Color levels in trichromic dye wastewater before and after UV/H2O2
treatment
In this aspect of the study, dye wastewater obtained from the initial
dyeing was subjected to a series of decolorization and reuse cycles for
cotton fabric dyeing. Results from the assessment of dye remaining in
trichromic dye wastewater reuse cycles are presented in Fig. 5. A com­
parison of dye wastewater generated by employing tap water and reused
water from dye wastewater treatments showed color remaining after UV/
H2O2 treatments gradually increased during successive dyeing, limiting
the practical reuse of the wastewater from reactive dyeing purposes to
three times.
According to the kinetics study carried out for trichromic wastewater
discoloration (Fig. S3, Supplementary data), the half-life was achieved
115 min. The pseudo-first-order model best fits the experimental data
(r2 = 0.096346, k1 = 0.00616 min− 1). The r2 value can be considered
rather good since the experiments were conducted with true wastewater
and instead of synthetic solutions. The experiments were conducted over
a 5 h period to ensure maximum discoloration before reuse.
3.2.2. Correction of conductivity in dye wastewater reused after UV/H2O2
treatment
The dye wastewater produced from reactive dye dyebaths can
exhibit high conductivity values. It is because the dyeing process em­
ploys electrolytes such as sodium chloride (salt) at concentrations that
can reach the order of 70 g/L depending on the dye used [48]. At the end
of our UV/H2O2 treatment, the wastewater had almost no reduction in
conductivity. This is consistent with the reported inability of AOPs
systems to remove salinity [49]. Bearing in mind that the reused
wastewater’s conductivity value is important during the subsequent
dyeing cycles, a method for calculating the amount of salt to add was
developed. Salt adjustments determined are recorded in (Table 1).
Table 1
Conductivity of dye wastewater before and after different reuse and treatment
cycles, and NaCl additions before a new dyeing cycle based on the conductivity
calibration curve, n = 3.
Cycle of Initial Conductivity Final Conductivity Salt Additions
treatment (ms/cm) (ms/cm) (g/L)
1st 2.421 ± 0.017 2.376 ± 0.079 63.62 ± 1.17
2nd 4.212 ± 0.014 4.183 ± 0.069 62.54 ± 0.21
3rd 8.064 ± 0.031 8.008 ± 0.078 60.31 ± 0.59
7
Journal of Environmental Chemical Engineering 9 (2021) 105731
Table 2
Total Organic Carbon (TOC) reduction from the different wastewater samples
obtained after dyeing/wastewater treatment cycles employing UV/H2O2.
Dye wastewater TOC content Samples originated by TOC content
used (mg/L) UV/H2O2 treatment (mg/L)
First dye
1186.0 1st treatment 8556.0
wastewater
Water from 1st
reused 4667.0 2nd treatment 26,500.0
wastewater
Water from 2nd
reused 7156.0 3th treatment 61,510.0
wastewater
Reusing the water with a simple salt adjusting can generate an economy
of salt employed in the dyeing process. Considering daily dyeing of
500 kg of fabric using a 1:10 bath ratio, totaling 5000 L of reused water,
it can be estimated an economy of 0.8 ton/mon (10 ton/yr). Besides, the
salinity of textile effluents is one of the major concerns of the textile
industry, the reuse of wastewater minimizes the quantities of salty water
to treat and dispose of, reducing effects on the environment.
3.2.3. Evaluation of TOC in dye wastewater before and after UV/H2O2
treatment
To characterize the effects of the UV/H2O2 treatment on water
quality, the Total Organic Carbon (TOC) of the initial and reused dye
wastewater was evaluated (Table 2). The UV/H2O2 treatment gave a
TOC reduction of 28% after the first wastewater treatment and 43% after
the second treatment. It was also found that after the third treatment,
the decrease of TOC content was 14%. It should be pointed out that TOC
reduction does not automatically mean that the dye molecules were
transformed into compounds with lower toxicity [49]. Following the
third treatment, the accumulation of dye residues and auxiliaries
contributed to the high TOC content. These results are in accordance
with the increase observed for color levels in trichromic dye wastewater
discussed in 3.2.1.
After the degradation process using H2O2/UV, there is a fraction of
organic matter that remains and is detected by TOC. Probably com­
pounds that are more resistant to the action of HO•. Therefore, the ef­
fluents treated and used for new dyeing processes carry the remaining
organic load that is more resistant to degradation. In the third waste­
water, the organic load contributes from the two previous cycles of
dyeing-treatment associated with the residues of dyes not melted into
the fabric from the third dyeing procedure. Since HO• is not selective
and presents a short half-life [50], it is probably that resistant organic
molecules act as obstacles for HO• to find more easily degradable,
leaving in solution residues of more resistant compounds from previous
treatments and those that originated from the third treatment cycle.
Such possibilities are suggested as hypotheses of the lower efficiency of
TOC reduction observed for the third wastewater treatment.
3.3. Assessment of cotton dyed with reused wastewater treated by UV/
H2 O 2
3.3.1. Coloristic properties
The color properties of the dyed cotton from the reused wastewater
samples were evaluated. The ΔE* values were determined using CIELAB
assessments; monochromic and trichromic dyeing results are presented
in Table 3. Where “L” corresponds to luminosity; axis “a” the differences
between green and red; “b” the differences between yellow and blue,
and “h” corresponds to the color tone.
In the Brazilian textile industry, ΔE* values in the 0.8–1.2 range are
generally acceptable [2]. Thus, the color differences measured for dyed
cotton fabrics obtained from the first and second reuse of wastewater
were acceptable as those obtained from dyeing employing tap water.
The experiment using the water from 2nd and 3rd wastewater treatments
K.C.H. Bezerra et al. Journal of Environmental Chemical Engineering 9 (2021) 105731

Table 3 from the 2nd wastewater treatment. Additionally, the sample dyed with
Color quality parameters for cotton fabric dyed using MCT/VS monochromic water from the 1st wastewater treatment was less reddish (∆a* = − 0.12)
and trichromic reactive dyes employing tap water and wastewater treated for and more yellow (∆b* = 1.43), while the sample dyed with water from
different times. *The experiments were not conducted for monochromic dye­ 2nd wastewater treatment was more reddish (∆ a* = 1.31) and slightly
baths since trichromic dyeing is more usual in the textile industry. more yellow (∆b* = 0.16).
Cotton dyed employing For the RED dye, the sample dyed with the 1st reused water showed a
Water Water reused Water reused minimal difference regarding luminosity (∆L* = 0.04). However, on the
Tap
Colorimetric reused from from 1st from 2nd and ∆a* axis, the differences were more significant, showing redness. For the
water
coordinates 1st reused and 2nd 3rd ∆b * axis, this difference was 0.21, indicating that the tissue sample is
control
treatment treatments treatments*
less bluish. For dyeing using water from the 2nd reuse, the differences in
YELLOW dyeing
∆L* , ∆a* , and ∆b* indicate that the dyed fabric is lighter and redder,
L* 74.71 74.50 74.32 – and less bluish.
a* 26.91 26.79 28.22
Concerning fabrics dyed with BLUE, an increase in luminosity was
–
b* 71.84 73.27 72.01 –
C* 76.72 78.01 76.63 – observed for the fabric dyed with the 1st reused water, denoting that this
h* 69.47 69.91 69.99 – is lighter when compared to the fabric dyed in tap water. Nevertheless,
∆L* - 0.21 - 0.39 – the values of ∆a* and ∆b* are minimum (− 0.07 and 0.06, respectively),
∆a* - 0.12 1.31 –
leading to the conclusion that only the luminosity was changed. For
∆b* 1.43 0.16 –
∆E* 0.62 0.58 – dyeing with the 2nd reused water, the value of ∆L denotes that the fabric
RED dyeing has become darker (ΔL* = 0.24), and the values of ∆a* and ∆b* suggest
L* 48.31 48.35 48.31 – that it has become less greenish and less yellow.
a* 58.20 58.75 58.20 – For fabrics dyed with a trichrome bath using reused water (Table 3),
b* -5.14 -4.92 -5.14
samples with the 1st reused water were slightly present clearer, reddish
–
C* 58.43 58.08 58.43 –
h* 354.95 366.21 354.95 – and yellowish according to the values of ∆L* , ∆a* , and ∆b* , respec­
∆L* 0.04 -0.62 tively. Considering the same parameters for the fabric dyed with the 2nd
∆a* 0.55 0.17 water for reuse, the sample showed the same changes: lighter, reddish,
∆b* 0.21 0.14
and yellowish. As it was possible to observe from the results obtained in
∆E* 0.24 0.35 –
BLUE dyeing the dyeing of the trichrome bath, the differences between axes L* , a* ,
L* 40.93 41.62 40.69 – and b* are very similar. The second sample presents a similar behavior
a* -0.74 -0.81 -0.48 – to the first, only observing a slight increase in color differences (∆E)
b* -30.84 -30.78 -31.85 – which changed from 0.25 to 0.47.
C* 30.85 30.79 31.83
However, for the fabric sample dyed with the 3rd cycle of reused
–
h* 268.62 268.49 269.69 –
∆L* 0.70 0.24 treated wastewater, ∆E suggested a considerable difference (2.28),
∆a* - 0.07 -0.26 which is not acceptable for the textile industry. The most significant
∆b* 0.06 + 1.01 difference was observed in the ∆b* axis (1.49), showing that the sample
∆E* 0.36 0.56 –
became bluer and less yellow. The parameters ∆a* (0.57) and ∆L* (0.40)
Trichromic dyeing
L* 40.5 40.3 40.8 40.0 suggest that the sample became redder and darker. This result indicates
a* 7.0 6.9 7.2 7.6 that it is more appropriate to carry out two cycles of dyeing and
b* 3.2 3.3 3.5 1.7 wastewater treatments. This conclusion is corroborated by TOC’s values
C* 7.7 7.6 8.0 8.2 that evidenced dissolved organic matter even after the UV/H2O2 treat­
h* 24.6 25.8 26.0 12.4
ments. It is important to note that the quality of the water after the 3rd
∆L* -0.14 0.30 0.40
∆a* -0.11 0.24 0.57 wastewater treatment does not prevent it from being used for other uses
∆b* 0.13 0.34 1.49 such as cleaning floors, toilets, as long as the composition of the
∆E* 0.25 0.47 2.28 remaining organic compounds is determined and that they do not pose a
risk to the environment and human health.
The experiments using the water reused from 2nd and 3rd wastewater
was not conducted for monochromic dyeing due to the dyeings using
treatments were not conducted for monochromic dyeing due to the
only one dye being rare in the textile industry. Fig. 6 present an image of
dyeing using only one dye being rare in the textile industry.
cotton fabrics obtained after the dyeing cycles exposed in Table 3. In
Fig. 6 is possible to check the similarity of the colors suitable for dyeing
3.3.2. Fastness properties
cotton fabric with the water from the sample treatment in different cy­
Colorfastness assessments were performed on the cotton fabrics dyed
cles. It is evident, even for the human eye, that the similarity of color was
in the reused wastewater to assess changes in the colors’ permanence
guaranteed for the first two reuses. As additional information, images of
and verify fastness reproducibility. The dyed fabrics were evaluated for
cotton fabric specimen dyed with trichromic bath are available as Sup­
fastness to light and washing. The wash fastness results are provided in
plementary Data (Fig. S4).
Table 4, where it can be seen that wash fastness was very good to
However, the magnitude of (ΔE) informs the real aspect of the total
excellent. It is also evident that dyeing using reused wastewater did not
difference between the dyed fabrics but does not indicate the character
have an adverse effect since the same fastness ratings were obtained for
of the differences between the colors. It does not indicate the relative
cotton dyed in the treated dyebath.
amount and direction of differences in brightness, chroma, and hue. This
The lightfastness results are presented in Table 5. The ratings were 5
information can only be obtained if each of the E components is
using the blue scale and 4 using the grayscale for color change. From
analyzed in isolation. It is necessary to evaluate the luminosity and the
these results, it was possible to conclude that reuse the effluent does not
values on the axes a* e b* [51].
adversely affect the quality of the dyed cotton since all the cotton dyed
For samples dyed with YELLOW bath, a slight darkening is observed,
with the reused wastewater showed the same rating as the control dyed
evidenced by the decrease in luminosity (∆L*) obtained from - 0.21 to -
cotton.
0.39 when using water from 1st wastewater treatment and water reused

8
K.C.H. Bezerra et al. Journal of Environmental Chemical Engineering 9 (2021) 105731

Fig. 6. Images of cotton fabrics after dyeing with monochromic or trichromic baths and employing water from different cycles of wastewater treatments and reuse.
The third reuse cycle was not conducted for monochromic baths since trichromic dyeing is more common in the textile industry.

4. Conclusions
Table 4
Wash fastness of cotton dyed in treated and reused wastewater after the tri­
Treating reactive dye wastewater using UV/H2O2 effectively
chromic dyeing.
removed color in samples containing residual azo and formazan MCT/
Color Transfer
Samples dyed in
Color VS dyes to levels permitting reuse of the treated water for subsequent
Change WO1 PAC2 PES3 PA4 CO5 CA6 dyeing cycles. The pH 4 level was optimal for color removal, and the
Control tap water 4/5 4/5 5 5 5 5 5 high conductivity of the decolorized wastewater did not impede its reuse
Water from 1st since salt is essential for the reactive dye application process. The quality
4/5 4/5 5 5 5 5 5
treatment cycle of cotton dyed with the first and second decolorized wastewater samples
Water from 1st
was acceptable for textile use, as the ΔE* values obtained were lower
reuse and 2nd 4/5 4/5 5 5 5 5 5
treatment cycles than 1.0. The fastness to light and washing was not adversely affected by
reusing the decolorized effluent, further validating the present AOP
1. WO: wool; 2. PAC: acrylic; 3. PES: polyester; 4. PA: polyamide (nylon); 5. CO:
treatment method’s utility.
cotton; CA: cellulose acetate. The rating scale was 1 (poor) to 5 (excellent).

Ethical approval
Table 5
Lightfastness of cotton dyed with reused wastewater after trichrome dyeing. Not applicable.
1 2
Sample Blue scale Gray scale
Consent to participate
Control 5 4
Cotton dyed with 1st reused wastewater 5 4
Not applicable.
Cotton dyed with 2nd reused wastewater 5 4

1. Blue scale: 1 (poor) to 8 (excellent). 2. Grayscale: 1 (poor) to 5 (excellent)

9
K.C.H. Bezerra et al.
Consent to publish
Not applicable.
Authors contributions
All authors contributed to the study’s conception and design. Mate­
rial preparation, data collection, and analysis regarding the steps dyeing
process, wastewater treatment with UV / H2O2, Total Organic Carbon
(TOC), quality assessments of cotton dyed in reused wastewater, fastness
testing were performed by [KCHB, SAC, SMC, GL, and HSF]. The first
draft of the manuscript was written by [KCHB, TRF, HSF, SMC, GL, and
SAC], and all authors read and approved the final manuscript. The
treatment and discussion of kinect data were done by [WDF].
Funding
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior –
Brasil (CAPES) - Financial Code 001- Post-doctoral scholarship from
Ticiane Rossi Fiaschitello.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data Availability
The datasets generated during and/or analyzed during the current
study are available in the [Katia Crystina Hipólito Bezerra] repository
[https://teses.usp.br/teses/disponiveis/100/100133/tde-09112015-
162713/publico/katiachbezerra.pdf]. DOI: 10.11606/D.100.2015.tde-
09112015–162713.
Acknowledgments
The authors acknowledge the Coordenação de Aperfeiçoamento de
Pessoal de Nível Superior – Brasil (CAPES) - Finance Code 001 for this
research’s financial support. The authors thank the School SENAI
Francisco Matarazzo (SENAI-SP) for the laboratory analysis support.
Appendix A. Supporting information
Supplementary data associated with this article can be found in the
online version at doi:10.1016/j.jece.2021.105731.
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