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Water Air Soil Pollut (2018) 229:92

Evaluation of Magnetic Coagulant (α-Fe2O3-MO) and its

Reuse in Textile Wastewater Treatment
Tássia Rhuna Tonial dos Santos & Gustavo Affonso Pisano Mateus &
Marcela Fernandes Silva & Carolina Sayury Miyashiro & Leticia Nishi &
Murilo Barbosa de Andrade & Márcia Regina Fagundes-Klen &
Raquel Guttieres Gomes & Rosângela Bergamasco

Received: 17 November 2017 / Accepted: 15 February 2018

# Springer International Publishing AG, part of Springer Nature 2018

Abstract The textile industries are characterized as one presence and absence of external magnetic field
of the biggest consumers of potable water and chemical (600 k Am−1). Kinetics sedimentation was from 0 to
products throughout its process, being responsible for 90 min. The use of this new coagulant allowed the
the elevated wastewater generation with intense colora- removal of 92.37% for apparent color, 91.43% for tur-
tion and wide polluting potential. In this context, the bidity, and 46.09% for UV254nm, indicating that the
present study proposes the development and application proposed coagulant association was efficient in the treat-
of a new coagulant material for textile wastewater treat- ment of this type of wastewater under external magnetic
ment. The proposed coagulant (α-Fe2O3-MO) was com- field with only 10 min of sedimentation. In addition, the
posed by hematite nanoparticles (α-Fe2O3) obtained by resulting sludge from CF process was tested as base
a simple non-pollutant methodology, associated with material for a new coagulant synthesis, demonstrating
Moringa oleifera (MO) seeds saline extract compounds. great reuse potential. Therefore, the new proposed co-
Coagulation/flocculation (CF) efficiency was evaluated agulant, composed of α-Fe2O3 and the compounds
by removal of physicochemical parameters such as ap- present in the seed extract of MO, has applicability for
parent color, turbidity, and compounds with absorption textile wastewater treatment demonstrating high remov-
at UV254nm (UV254nm) through CF tests carried out on al rate for all evaluated parameters with cost reduction in
Jar test equipment and sedimentation carried out in the the proposed treatment for this wastewater.

T. R. T. dos Santos : M. F. Silva : L. Nishi :

Keywords Hematite . Moringa oleifera . Magnetic
M. B. de Andrade : R. Bergamasco (*) sedimentation . Textile wastewater
Department of Chemical Engineering, Universidade Estadual de
Maringá, Avenida Colombo, 5790, Bloco D90, Maringá, Paraná
CEP: 87020-900, Brazil
e-mail: 1 Introduction

G. A. P. Mateus Water is one of the most abundant natural resources on

Department of Biotechnology, Genetics and Cell Biology, Earth; however, only a small portion of this supply is
Universidade Estadual de Maringá, Maringá, Paraná, Brazil
available for human consumption, especially regarding
C. S. Miyashiro : M. R. Fagundes-Klen potable water source contamination, high cost treatment,
Department of Chemical Engineering, Universidade Estadual do increasing population demand, and the wide variety of
Oeste do Paraná, Toledo, Paraná, Brazil organic and inorganic emerging pollutants involved in
R. G. Gomes different production processes (Adeleye et al. 2016).
Department of Food Engineering, Universidade Estadual de In this sense, the treatment and reuse of wastewater
Maringá, Maringá, Paraná, Brazil have become relevant subjects in terms of sustainability
92 Page 2 of 17 Water Air Soil Pollut (2018) 229:92

(Lu and Leung 2003). Recently, several reuse techniques potential, excessive exposure to highly colored waste-
began to be widely diffused in urban, agricultural, and waters can cause disturbances in respiratory, circulatory,
industrial environments (Lazarova et al. 2000) highlight- and central nervous systems (Foo and Hameed 2010).
ing the relevance of new technologies for natural water The available literature presents several conventional
sources preservation (López-Ramírez et al. 2006). methods for textile wastewater treatment involving pro-
The textile industries stand out as one of the largest cesses such as ion exchange, membrane filtration, pre-
consumers of potable water and chemical agents to carry cipitation, flotation, solvent extraction, adsorption, co-
out their processes, generating wastewaters of complex agulation/flocculation, and biological methods (Radoiu
composition and high coloration, turbidity, and chemi- et al. 2004). However, none of these methods alone is
cal and organic load (Verma et al. 2012). This wide economically feasible and efficient for color removal of
characteristic variation in textile wastewater can be at- textile industry wastewater and usually needs to be
tributed to the complexity of used materials and differ- associated with another method to achieve satisfactory
ent processes that occur in textile industries. efficiency (Robinson et al. 2001).
Wastewater from textile industries may contain dif- Good color removals were achieved by several re-
ferent types of dyes, which provides residues with high searchers around the world, using a wide range of raw
molecular weight, especially due to the complex struc- and synthetic textile wastewater. However, all the ap-
tures of these dyes. Due to the amount of chromophores plied methods present some limitations, as the compli-
and auxochromes, these residues have a varied compo- cated regeneration and high costs for final adsorbent
sition and low biodegradability (Gao et al. 2007) being disposal stand out, in case of adsorption (Hai et al.
responsible for dyes’ color intensity (Christie 2001). 2007; Robinson et al. 2001) and production of concen-
Other substances may also be present in this type of trated sludge and high operating costs regarding mem-
wastewater, such as cleaning solvents, inorganic salts, brane filtration (Marcucci et al. 2001; Arbari et al.
waste from the preparation, dyeing and finishing pro- 2006). In general, the efficiency of conventional dye
cesses, and a complex mixture of chemical reagents removal processes becomes limited as the concentration
(USEPA 1997; Babu et al. 2007; Debik et al. 2010; and solubilization of dyes increases (Zahrim et al. 2010).
Ciabatti et al. 2010). The association of these factors The CF process is observed as one of the most
and these peculiar characteristics makes treatment and practiced method for wastewater remediation, and it is
color removal of this type of wastewater a major used as treatment or pretreatment, mainly due to its low
challenge. cost, making this process an interesting alternative, par-
The inadequate disposal of these wastewaters can ticularly for developing countries (Golob et al. 2005),
result in several environmental impacts, among them which stand out for the high textile wastewater genera-
the color change in aquatic environments that hinders tion. The CF process for wastewaters involves the addi-
light penetration into water, causing and accelerating the tion of chemical agents to the solution, seeking to alter
eutrophication process, consuming dissolved oxygen, the physical state of the suspended and dissolved solids,
and hindering water reoxygenation, besides being toxic facilitating its removal by gravitational sedimentation.
to aquatic life (Georgiu et al. 2003; Ustun et al. 2007; However, this process presents disadvantages like the
Foo and Hameed 2010). The discharge of dye- high sedimentation time required, besides using inor-
containing effluents without adequate treatment is a ganic coagulants such as aluminum salts, which pro-
matter of serious concern not only for the undesirable mote environmental problems and implications for hu-
visual pollution associated with the color in wastewater man health (Wang et al. 2012).
but also by the negative impacts on the environment, Based on this problem, an intensive research effort
such as inhibition of aquatic photosynthesis, reduction has been made worldwide to develop an effective, eco-
of water reoxygenation capacity, depletion of dissolved nomically viable, and eco-friendly replacement for the
oxygen, and acute and chronic toxicity affecting flora, conventional coagulants and flocculants currently used
fauna, and humans (Martinez-Huitle and Brillas 2009; by different industries with high pollution potential
Rodríguez-Couto 2015; Ortiz-Monsalve et al. 2017). (Sharma et al. 2006). Among the recently researched
This type of wastewater still represents great risks for alternative coagulants, Moringa oleifera (MO) attracts
groundwaters (Khaled et al. 2009) and also for human attention (Nand et al. 2012), due to the coagulant prop-
health. In addition to carcinogenic and microtoxic erty of its seeds, provided by cationic proteins adequate
Water Air Soil Pollut (2018) 229:92 Page 3 of 17 92

for clarifying surface and residual waters and precipitat- Table 1 Textile raw wastewater characterization
ing organic and mineral particles from a solution Parameters Values Analysis method
(Rockwood et al. 2013).
Another field that has been actively contributing to Apparent color (uH)a 707.3 Spectrophotometer Hach
the development of new wastewater treatment methods model DR/2000
is nanotechnology (Anjum et al. 2016). Recently, mag- Turbidity (NTU)b 128 Policontrol turbidimeter
model AP2000
netic nanoparticles have been tested for heavy metals
UV254nm (cm−1) 0.640 Spectrophotometer Hach
and hazardous materials removal from water (Rajput
model DR/2000
et al. 2016). Magnetic nanoparticles have unique and
pH 3.27 pH meter—Digimed
favorable characteristics in relation to their use, such as
Zeta potential (mV) − 8.49 Beckman Coulter
low cost and toxicity, high magnetism, durability and Delsa™ Nano Zeta
biocompatibility (Laurent et al. 2008), and easy separa- Potential Analyzer
tion from aqueous solutions (Medvedeva et al. 2015).
Analysis method performed according to Standard Methods
The biocompatibility of these materials makes their (APHA 2005)
association with biological compounds a promising al- a
Hazen unit = (mg Pt-Co L−1 )
ternative for several applications as treatment of water b
Turbidity unit
supply (Santos et al. 2016; Gupta et al. 2015) or indus-
trial wastewaters (Brumfiel 2003).
The spectrum obtained from EDX analysis is shown
Considering the above mentioned, the objective of
the present study was to evaluate the efficiency of the in Fig. 1. The compounds present in the raw wastewater
association between magnetic nanoparticles (α-Fe2O3) are frequent due to the dye compounds commonly used
and compounds present in MO seeds for raw textile in the textile industry (Verma et al. 2012) and the other
wastewater treatment. The developed magnetic coagu- products involved throughout washing process, for ex-
lant was evaluated in relation to removal efficiency of ample Na, Ca, S, and Si.
quality physicochemical parameters such as apparent
color, turbidity, and compounds with absorption at 2.2 Magnetic Nanoparticle Synthesis
UV254nm. In addition, studies on the mechanisms in-
volved in the CF process as well as settling kinetics The nanoparticles composed by hematite phase of iron
and coagulant reuse were also performed. oxide were synthesized by a modified aqueous sol–gel
method according to Pastor et al. (2012). Iron nitrate
aqueous solution was mixed at room temperature under
2 Materials and Methods stirring for 2 h and then heated until complete water
evaporation. After these procedures, the residue was
2.1 Textile Wastewater Samples calcined at 400 °C for 4 h in muffle.

Raw textile wastewater samples were collected in the 2.3 Nanoparticle Characterization
entrance of the textile treatment plant situated in Pérola
city, located in the northwest of Paraná State, Brazil. The crystalline structure of the nanoparticles was identi-
Before the analytical procedures, their characteristics fied by X-ray diffraction (XRD) data using a Siemens D-
were evaluated for apparent color, turbidity, zeta poten- 5000 powder diffractometer with monochromated Cu–
tial, and compounds with absorption at UV254nm whose Kα radiation (λ = 1.54056 Å). The XRD was measured
results are shown in Table 1. The wastewater was also in the range between 25 and 60° in 2θ. The size of the
characterized in relation to the elemental composition, crystallites synthesized were estimated using Scherrer’s
by using energy-dispersive X-ray spectroscopy (EDX) Eq. (1), in which 0.89 is the Scherrer constant, λ is the
(Fig. 1), performed on Quantum 250 (FEI) equipment wavelength, B is the full width at half maximum
coupled with Spectra Software AZtec 3.0 EDX (Oxford (FWHM) of the peak, and cosθ is the Bragg angle.
Instruments Nanotechnology Tools Ltd). This wastewa-
ter was used for coagulation/flocculation/sedimentation 0:89λ
d¼ ð1Þ
(CFS) assays, using magnetic coagulant. ðBcosθB Þ
92 Page 4 of 17 Water Air Soil Pollut (2018) 229:92

Fig. 1 Raw textile wastewater

elementary composition obtained
by EDX

The morphology were examined using a 120-kV 2.6 Preparation of Magnetic Coagulant
JEOL JEM-1400 transmission electron microscope
(TEM). The hematite powders were characterized by The magnetic coagulant was prepared according to the
infrared spectroscopy (FTIR) using a FTIR-BOMEM- methodology proposed by Santos et al. (2016), with
100 Spectrometer using KBr pellets. The magnetization some modifications. Therefore, 20 mL of MO saline
measures as function of applied magnetic field (− 60 to extract (200, 400, 600 mg L−1) (Madrona et al. 2010;
60 kOe) at 100 and 300 K were performed on a vibrating Santos et al. 2016) and different amounts of α-Fe2O3
sample magnetometer (VSM-2T; Lakeshore). (40, 60, or 80 mg) were stirred by ultrasound for 5 min
The scanning micrograph of α-Fe2O3 was performed (min). The mixtures (MO saline extract + nanoparticles)
on a Quanta 250 (FEI) electronic microscope (SEM) and were stirred at room temperature for 1 h. Each associa-
elemental composition analysis was performed on the tion was designed by different letters, as shown in
same equipment coupled with Spectra AZtec 3.0 EDX Table 2.
support software (Oxford Instruments Nanotechnology
Tools Ltd) for X-ray spectroscopy by energy dispersion. 2.7 Magnetic Coagulant Characterization

2.4 Moringa oleifera Seed Preparation The magnetic coagulant were characterized by zeta po-
tential varying the pH values from 2 to 12, by electro-
Mature MO seeds were provided by Universidade Fed- phoretic light dispersion using the equipment Beckman
eral de Sergipe (UFS), Aracaju—SE, Brazil. These Coulter DelsaTM Nano Zeta Potential Analyzer. The
seeds were stored under refrigeration so their original EDX composition was performed according to the
characteristics could be maintained till the analytical methodology described in BTextile Wastewater
procedures. The seeds were then peeled and crushed. Samples^ section.

2.5 Preparation of MO Saline Extract 2.8 Jar Test Assays

One gram of crushed seed was mixed with 100 mL Experimental tests were conducted in the jar test equip-
of NaCl aqueous solution (1 mol L−1) under mag- ment (Nova Ética Model-218LDB) with 300 mL of raw
netic stirring for 30 min (Madrona et al. 2010). The textile wastewater into recipients of 600 mL capacity.
MO active principle was extracted by salting-out The CFS efficiency was determined by the removal
mechanism, responsible for increasing the ionic capacity of apparent color, turbidity, and UV254nm, cal-
strength and solubility of the active components, culated by Eq. (2), where Ci and Cf are the initial and
improving the coagulant capacity of MO seeds final values, respectively, for each parameter:
(Okuda et al. 2001). Afterwards, this mixture was vac-
uum filtered on a qualitative membrane, obtaining 1%  
(considering initial mass) of saline extract (Madrona Ci−C f
%Removal efficiency ¼ 100 ð2Þ
et al. 2010). Ci
Water Air Soil Pollut (2018) 229:92 Page 5 of 17 92

Table 2 Different treatment composition (MO saline extract and nanoparticles association)

Treatment A B C D E F G H I J K L

α-Fe2O3 (mg) 0 0 60 40 40 40 60 60 60 80 80 80
MO (mg L−1) 0 400 0 200 400 600 200 400 600 200 400 600

For the CFS process, the following conditions were 3 Results and Discussion
applied: coagulant doses of 200, 400, and 600 mg L−1;
rapid mixing rate (RMR) of 100 rpm for 2 min; and 3.1 Iron Oxide Characterization
slow mixing rate (SMR) of 20 rpm for 20 min (Golob
et al. 2005), after coagulation/flocculation a total In relation to elemental composition (EDX), the obtain-
sedimentation time of 30 min was applied; however, ed iron oxide nanoparticles (Fig. 2) present only Fe and
the removal efficiency for the proposed coagulant O, similar to those obtained by Zayed et al. (2017) using
was evaluated at times 10, 20, and 30 min, in the another method for the synthesis of α-Fe2O3 indicating
absence and under external magnetic of 600 k Am−1 that the synthesis method used allows obtaining such
measured using Gaussmeter equipment (Lakeshore, materials without impurities.
425 Gaussmeter) in order to evaluate the influence of The obtained iron oxide was characterized related to
magnetic sedimentation. crystalline structure by XRD, presented functional
chemical groups by FTIR, magnetic properties by mag-
2.9 Sedimentation Kinetics netization as function of magnetic applied field and
temperature, and morphological structure by TEM and
Jar test assays were performed in order to verify the SEM. The structure as well as the average crystallite size
required time of sedimentation. The settling time ranged were analyzed using X-ray diffraction (Fig. 3). The
from 0 to 90 min. The samples were collected at times 3, obtained diffraction pattern are in perfect agreement
5, 10, 20, 30, 45, 60, 75, and 90 min, being evaluated for with the standard JCPDS 87-1166 of hematite (α-
removal efficiency of apparent color, turbidity, and Fe2O3). At room temperature, hematite phase is weakly
UV254nm, for each sedimentation time. ferromagnetic. The estimated crystallite diameter by
Scherrer’s equation (33° peak) was nearly 40 nm, in
2.10 Refunctionalized Sludge agreement with previous studies using the same synthe-
sis method to obtain nanosized particles (Pérez-
For the reuse assays, the resulting sludge of the CFS Landazáball et al. 2015).
process, containing magnetic nanoparticles, were Figure 4 shows the FTIR spectrum of obtained iron
dried at 70 °C for 1 h. After drying the sludge, this oxide. The bands in the range of 750–400 cm−1 are
resulting material was again functionalized with the related to Fe–O lattice vibration. Hematite phase pre-
compounds present in the MO extract, according to sents bands at 620, 540, and 470 cm−1, but the positions
the methodology described in the BPreparation of of the bands are sensitive to the particles size and shape
Magnetic Coagulant^ section giving rise to a new (Gotic and Music 2007; Pedroi 2007).
coagulant. This spectrum presents no bands except Fe–O link-
This coagulant was then used for new CFS ages, indicating the absence of impurities or humidity,
assays. The evaluation of removal parameters was according to EDX results. It is probably due to non-use
performed using the same conditions of the opti- of organic capping agents, as polymers or organic mol-
mum treatment found in previous CFS assays. The ecules, but only water and metal precursor in the syn-
coagulant regeneration potential was studied in two thesis method.
successive reuses and characterized in relation to As it can be appreciated in the micrograph obtained
the elemental composition obtained by EDX, ac- by TEM (see Fig. 5), nanoparticles have a round shape.
cording to the methodology described in BTextile According to Sadykov et al. (2000), if iron oxides are
Wastewater Samples^ section. obtained through decomposition of a nitrate salt
92 Page 6 of 17 Water Air Soil Pollut (2018) 229:92

Fig. 2 Iron oxide elementary

composition obtained by EDX

solution, the particles are usually elongated, round are not in a rigid antiparallel arrangement. There is a
shaped, and contain few extended defects. The rounded slight canting angle between the Morin temperature
surface nanoparticles implies presence of high index (240 K) and the Neél temperature (948 K) (Kihal
stepped faces, on which the terminal oxygen species et al. 2009). The magnetic phase transition (Morin
bound to the regular cations may appear. The size of transition) at about 240 K (Pérez-Landazáball et al.
the nanoparticles from the image is similar to the one 2015), followed by a decrease in magnetization, also
obtained by X-ray diffraction. It could be observed that leads to a Bcollapse^ of the hysteresis curve. Before
nanoparticles present as agglomerates due to the ferro- the transition, at T = 300 K, the coercive force was
magnetic characteristics of the obtained material. Fig- H c = 3.19 kOe. Upon cooling, the structure un-
ure 6 shows the SEM micrograph of α-Fe2O3, and it is dergoes a first order spin reorientation, in which the
possible to note that particles are present as aggregates net magnetic moment is lost and after the transition,
formed by nanometric particles, being in agreement at T = 100 K, the coercive force Hc = 160 Oe. As
with TEM micrographs. shown, saturation is not reached up to the maximum
The magnetization were studied in function of ap- applied magnetic field, similar to a previous report by
plied magnetic field (at T = 300 K and T = 100 K), as Peng et al. (2010). The magnetic behaviors of hema-
shown in Fig. 7. There is a hysteretic behavior in low tite depend on crystallinity and particle size. It is
fields since hematite can present a weak parasitic ferro- known that coercivity is influenced by several possi-
magnetism because the electron spin magnetic moments ble factors, such as size, structure, surface disorder,

Fig. 3 XRD diffractogram of

obtained iron oxide
Water Air Soil Pollut (2018) 229:92 Page 7 of 17 92

Fig. 4 FTIR spectrum of

obtained iron oxide

morphologies, etc. Lower crystallinity may be the main and α-Fe2O3-MO with the pH variation in order to aid in
reason for the high coercive force presented in this understanding the possible involved mechanisms
study, compared to that previously reported in literature (Fig. 8).
(Peng et al. 2010; Özdemir and Dunlop 2014). As observed in Fig. 8, among the three materials
analyzed, MO and α-Fe2O3 exhibit similar behavior,
3.2 Magnetic Coagulant Characterization being positively charged at pH below than 6.70 and
negatively charged at pH above this value. However,
The magnetic coagulant was characterized by potential the iron oxide presents an amphoteric behavior, variable
zeta and EDX and the results are shown below. The zeta according to the concentration of protons or hydroxyls
potential analysis was performed to obtain information in the solution. The coagulant α-Fe2O3-MO presents
about the surface electrostatic charge of MO, α-Fe2O3, zero potential charge at pH 9.27 and is positively
charged at values below than this.
According to Verma et al. (2012) most of the dyes
present in wastewaters from textile industries are nega-
tively charged; therefore, cationic compounds are pref-
erable for the treatment of these residues, a fact that
corroborates the use of the coagulant obtained in the
present study constituted in part by cationic proteins
(Baptista et al. 2015), responsible for the coagulant
potential of MO seeds.
In relation to the elemental composition of the coag-
ulant α-Fe2O3-MO, expressed in Fig. 9, it is possible to
observe the presence of α-Fe2O3 and MO compound
elements, indicating that the association becomes
The presence of the elements Na and Cl is related
to saline extraction of the compounds present in the
seeds of MO, which according to Ndabigengesere
et al. (1998) and Okuda et al. (2001) increase the
ionic strength and solubility of the active compounds
Fig. 5 Micrograph of synthesized iron oxide obtained by TEM present in the seeds.
92 Page 8 of 17 Water Air Soil Pollut (2018) 229:92

Fig. 6 Micrograph of
synthesized iron oxide obtained
by SEM

3.3 Jar Test Assays 91.43%, and for UV254nm the removal (Fig. 12) reached
46.09%. Removal values of 87.45% for apparent color,
The magnetic coagulant was tested in order to evaluate 86.42% for turbidity, and 42.63% for UV254nm were
which coagulant combination present better removal obtained using the same treatment in the absence of a
efficiency for the evaluated parameters, under and in magnetic field, demonstrating that presence of the mag-
the absence of external magnetic field, in sedimentation netic field assists in the removal of evaluated physico-
times of 10, 20, and 30 min. chemical parameters, as observed in Figs. 10, 11, and
Regarding removal efficiency for all evaluated pa- 12, respectively.
rameters, the greatest results were achieved by α-Fe2O3- Regarding MO dosage, 400 mg L−1 was the concen-
MO coagulant, using H treatment (60 mg L−1 of α- tration that presented the best removal of the physical–
Fe2O3 and 400 mg L−1 of MO) under applied magnetic chemical parameters evaluated. These results are in
field after 10 min of sedimentation. In relation of appar- accordance with previous studies by Santos et al.
ent color removal (Fig. 10), it achieved 92.37% of (2016) in which functionalized nanoparticles with MO
removal; for turbidity (Fig. 11), the removal was extract were used to remove the same parameters

Fig. 7 Magnetization versus

magnetic applied field curves at
100 and 300 K
Water Air Soil Pollut (2018) 229:92 Page 9 of 17 92

Fig. 8 Zeta potential versus pH

of iron oxide nanoparticles α-
Fe2O3, MO saline extract, and
magnetic coagulant α-Fe2O3-MO

evaluated in the present study, what exalts the use of this internal magnetic moment spinning in the same direc-
coagulant since the specified dosage is the same needed tion of the external magnetic field. This fact increases
when using synthetic and non-magnetic coagulants, the nanoparticles’ magnetic properties (Lu et al. 2007;
such as magnesium chloride and ferrous sulfate (Tan Okoli et al. 2012).
et al. 2000; Georgiu et al. 2003) obtaining removals of The use of the two compounds (MO and hematite)
apparent colors of 85 and 90%, respectively. Besides for dye removal is also reported in some studies. Sajjadi
that, several studies using alum-based coagulants report and Goharshadi (2017) evaluated hematite for methy-
apparent color removal lower to the one obtained in the lene blue and rhodamine removal achieving good effi-
present study (El-Gohary and Tawfik 2009; Kumar et al. ciency. In another study, biosynthesized nanoparticles of
2008; Patel and Vashi 2010; Bidhendi et al. 2007; hematite could effectively remove hazardous pollutants
Suksaroj et al. 2005; Tun et al. 2007; Selkuc 2005). from water including methyl red and eosin yellowish
The association of magnetic nanoparticles with the (Rufus et al. 2017).
compounds present in MO seeds saline extract results in Ströher et al. (2012) evaluated the removal of color
magnetic coagulation with characteristics of both mate- and turbidity of an effluent from jeans washing using the
rials, facilitating the impurities’ sedimentation through natural coagulant MO (1400 mg L−1) after treatment
the aggregation of this in magnetic flakes, which while removals greater than 80.33% for color and 91.10%
being exposed to an external magnetic field have the for turbidity were achieved.

Fig. 9 α-Fe2O3-MO coagulant

elementary composition obtained
by EDX spectra
92 Page 10 of 17 Water Air Soil Pollut (2018) 229:92

Fig. 10 Apparent color removal over time (10, 20, and 30 min) in the presence and absence of external magnetic field

Congo red and tartrazine could be removed with adsorption due to the anionic action of the coagulant
good efficiency using MO seeds according to Patel (positively charged) causing reduction of the existing
and Vashi (2012) and Reck et al. (2018). surface charges. In addition, adsorption and charge
The positive zeta potential of isolated MO suggests neutralization refer to sorption of oppositely charged
that the mechanisms involved in the coagulation and ions (Verma et al. 2012).
flocculation process are charge neutralization and ad- Couto Jr et al. (2013) investigated the CF for treating
sorption (Mangale et al. 2012); therefore, the similar effluents of textile industry using chemical coagulant
zeta potential behavior of magnetic coagulant and iso- aluminum sulfate and natural coagulant tannin. The
lated nanoparticles indicates that possibly the same percentage of removal, according to the best optimiza-
mechanisms are involved. tion test, was 93.12, 99.06, and 99.29% for COD, color,
Both the adsorption and coagulation processes are and turbidity, respectively, using the coagulant alumi-
individually efficient for the removal of compounds num sulfate, and 94.81, 99.17, and 99.65% for COD,
that impart color to textile wastewaters (Papic et al. color, and turbidity, respectively, using the coagulant
2000; Robinson et al. 2001; Papic et al. 2004). Ac- tannin.
cording to Bongiovani et al. (2014), the coagulation Sequencing coagulation (with AlCl3) and photo-
and flocculation process involves two mechanisms, catalytic degradation using UVA/MgO nanoparticles
the first being the destabilization of the colloidal process was investigated for the removal of COD
system by chemical interactions between the coagu- from raw effluent of a textile factory, achieving
lant molecules and the compounds present in the yielded considerable total COD removal of 98.3%
textile wastewater (negatively charged anionic, with (Jorfi et al. 2016)
zeta potential of − 8.49). Secondly, a complex of Therefore, in view of the obtained information from
coagulant and wastewaters compounds is formed by CFS assays and zeta potential behavior, it is possible to
Water Air Soil Pollut (2018) 229:92 Page 11 of 17 92

Fig. 11 Turbidity removal over time (10, 20, and 30 min) in the presence and absence of external magnetic field

infer that the mechanism involved in the process are 3.4 Settling Kinetics
composed of combined mechanisms such as charge
neutralization and adsorption (Kim et al. 2004; Lee The sedimentation kinetics were performed using the
et al. 2006). In addition, the presence of saline com- best treatment obtained in the CF step (treatment H—
pounds usually causes compression of the double layer, 60 mg of α-Fe2O3 and 400 mg L−1 of MO), under the
resulting in the destabilization of the particles in the same operating conditions as described previously
wastewater over electrostatic repulsion interactions, be- (RMR of 100 rpm for 2 min and SMR of 20 rpm for
ing attracted by the forces of Van der Waals (Sulaiman 20 min). The results are shown in Fig. 13.
et al. 2017). As shown in Fig. 13, in the early sedimentation
The results obtained in the present study demon- minutes, elevated removals were obtained, without sig-
strates that the coagulant used is characterized as an nificant increases in removals after 10 min (92.37% for
efficient alternative for textile wastewater treatment, apparent color, 91.43% for turbidity, and 46.09% for
especially due to the reduced time of sedimentation UV254nm), demonstrating that 10 min is a sufficient time
necessary for satisfactory removals of the physical– to obtain satisfactory results when compared to the
chemical parameters analyzed. Considering the sat- following times (whose difference would not be signif-
isfactory results obtained by the treatment H icant at a level of 5%).
(60 mg of α-Fe2O3 and 400 mg L−1 of MO), it Other studies using only MO as a coagulant to treat
was chosen for the realization of the complementa- different wastewaters required 20 min (Ströher et al.
ry studies, like the kinetics of sedimentation and 2012) and 60 min (Mateus et al. 2017a, 2017b) of
the reuse of the residual material formed after the sedimentation to remove the quality parameters in
new refunctionalization. actual wastewaters from the textile and the dairy
92 Page 12 of 17 Water Air Soil Pollut (2018) 229:92

Fig. 12 UV254nm removal over time (10, 20, and 30 min) in the presence and absence of external magnetic field

industries, respectively, differing from the time found in with the compounds present in the saline extract of
the present study, in which 10 min of sedimentation MO increased the efficiency of removal of the eval-
was enough to obtain satisfactory results, demon- uated parameters and allowed a reduction of sedi-
strating that the presence of nanoparticles associated mentation time.

Fig. 13 α-Fe2O3-MO settling

kinetics in the presence of
external magnetic field
Water Air Soil Pollut (2018) 229:92 Page 13 of 17 92

Fig. 14 Removal parameters of

apparent color, turbidity, and
UV254nm in CFS process using
refunctionalized sludge using
treatment H (60 mg α-Fe2O3 and
400 mg L−1 of MO) under
external magnetic field

3.5 Refunctionalized Sludge reuse was of 90.81% for apparent color, 90% for
turbidity, and 43.64% for the UV254nm, presenting
The sludge reuse assays were performed using resulting similar efficiency in this first use (92.37% removal
sludge of CFS process for two consecutive times, fol- of apparent color, 91.43% for turbidity, and 46.09%
lowing the conditions applied on the optimal treatment for UV254nm). A possible reason for removal effi-
found in previous CFS tests (60 mg of α-Fe2O3 and ciency had been maintained after the first sludge
400 mg L−1 of MO). Therefore, the resulting sludge refunctionalization by the compounds present in
containing nanoparticles was again associated to MO MO saline extract that they do not alter the electro-
saline extract, following the methodology previously static energy involved in the interaction among the
described. After new CFS tests with refunctionalized components of the coagulant (Okoli et al. 2012).
sludge as coagulant, the removal efficiencies were cal- Another possibility consists of functional groups
culated and the results are expressed in Fig. 14. disponibilization by the new refunctionalization with
Regarding the results expressed in Fig. 14, it is soluble compounds present in MO saline extract
possible to observe that the refunctionalized sludge which makes its efficiency very similar to the effi-
presents great reuse potential, confirmed through ciency obtained of the first use.
obtained results after the first refunctionalization Furthermore, as expressed by EDX, in the sludge
and use in new CFS test. The removal after the first from the first reuse (Fig. 15), the common elements to

Fig. 15 Elementary composition

of resulting sludge from the first
reuse obtained by EDX spectra
92 Page 14 of 17 Water Air Soil Pollut (2018) 229:92

Fig. 16 Elementary composition

of resulting sludge from the
second reuse obtained by EDX

the textile wastewater as well as the constituent elements the treated wastewater obtained suitable for indirect
of the magnetic coagulant are in large quantity in the industrial reuse.
waste material.
In the second reuse, the removals obtained were
79.90% for apparent color, 80% for turbidity, and 4 Conclusion
36.82% for UV254nm. The most probable reason for
the reduction in coagulant activity after the second In this study, the removal of apparent color, turbidity,
reuse consists of the increase of elements such as C, and UV254nm was investigated using MO soluble
S, Na, and Cl in the sludge, being C and S common in compounds and α-Fe2O3-MO in CFS process of tex-
chromosphore composition, elements of high stain- tile wastewater in the presence and in the absence of
ing present in the textile dyes (Christie 2001); Cl and external magnetic field. It was possible to observe
Na originate from the extraction method of MO com- that the composite material presented the best removal
pounds present, according to elemental analysis efficiencies, reaching values of 92.37% for apparent
expressed in Fig. 16. Another fact that must be ob- color, 91.43% for turbidity, and 46.09% for UV254nm,
served is the reduction of the percentage of the ele- indicating that the proposed association was efficient in
ments Fe and O, common to the iron oxide and the treatment of this type of wastewater; in addition, it
present in the carbonyl, carboxylic acid, and amide was possible to obtain high removals with reduced
groups, available in soluble extracts of MO (Tavares sedimentation time when submitted to magnetic field,
et al. 2017). differing from other treatments which require a high
The result sludge allowed new functionalization sedimentation time.
and application in new CFS assays leads to a poten- Reuse studies demonstrated the possibility of
tial coagulant material economy and effective reduc- sludge destination as a component of new coagulant
tion in the produced sludge (Golob et al. 2005), material, which presented similar removal efficiency
reducing inherent costs to the process. Besides, an- as its first use, reducing sludge generation and con-
other advantage related to natural products-based sequently reducing expenses with the final disposal
coagulants use is the reduction in formation of sub- of this material, resulting in a reduction of costs in the
products even more harmful to the environment and process.
to human health (Verma et al. 2012). Therefore, the new proposed material composed of
In this sense, the proposed coagulant can be con- α-Fe2O3-MO and the compounds present in MO seed
sidered as an effective coagulant for this type of extract have applicability for textile industry wastewater
wastewater, especially because the residue generated treatment, demonstrating high removals for all evaluat-
in the CFS process (composed by MO and α-Fe2O3) ed parameters, characteristics that are favorable and
is biodegradable and common to soil composition. consistent with environmental issues.
For reuse purposes, the association of treatments can
be an alternative to the conventional treatments used Acknowledgments The authors thank the financial support of
for treating wastewater from textile industry, being CAPES and Fundação Araucária.
Water Air Soil Pollut (2018) 229:92 Page 15 of 17 92

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