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Keywords: A novel pilot-scale hydrodynamic cavitation (HC) reactor was used to decolorize industrial-grade dye solutions
Hydrodynamic cavitation and printing ink wastewater (PIW). The effect of the orifice plate geometry (1 hole plate of 1 mm and 2 mm in
Pilot-scale reactor diameter, 31 holes of 1 mm and 2 mm in diameter, 62 holes of 1 mm and 2 mm in diameter), inlet pressure (4, 5
Venturi tube and orifice plate
bar), initial dye concentration (0.3 and 0.6 OD), and the synergistic effect of HC and hydrogen peroxide con
Color removal
centration (0.0, 0.5, 1.0, 2.0 g/L) were investigated. The results showed that the highest color removal was
COD removal
Wastewater treatment obtained using 31 holes orifice plate of 2 mm holes’ diameter, at 4 bar inlet pressure. Furthermore, although HC
could not degrade completely all the industrial-grade dyes, efficiency was enhanced in the presence of H2O2. The
optimum concentration of hydrogen peroxide was 1.0 g/L regardless of the initial concentration of the dyes
studied. Under optimum operating conditions, color removal reached up to 68% for black, 39% for red, 43% for
yellow, 55% for green, and 51% for cyan dye, while color removal in the PIW reached only 15%. The black dye
solution presented almost 100% COD removal, while 38%, 25%, 67%, and 78% COD removal values were ob
tained for the red, yellow, cyan and green dyes, respectively. 55% COD removal was recorded from the PIW.
Concerning cavitation yields, black, red, yellow, green, cyan dye yields reached 2.5E(-7), 1.1E(-7), 1.5E(-7), 2.0E
(-7), 1.7E(-7) OD⋅L/J, respectively, while PIW yield was 6.3E(-8) OD⋅L/J. The present study demonstrates that
HC combined with green oxidants such as hydrogen peroxide could be an alternative treatment approach for real
industrial wastewater streams. However, a combination with a post-treatment method should be applied to
maximize both color and COD removal.
* Corresponding author. Department of Chemical Engineering, University of Patras, Rio, GR-26504 Patras, Greece.
E-mail address: dvagenas@upatras.gr (D.V. Vayenas).
https://doi.org/10.1016/j.jenvman.2021.113301
Received 31 May 2021; Received in revised form 12 July 2021; Accepted 13 July 2021
Available online 16 July 2021
0301-4797/© 2021 Elsevier Ltd. All rights reserved.
C. Zampeta et al. Journal of Environmental Management 297 (2021) 113301
Nomenclature
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C. Zampeta et al. Journal of Environmental Management 297 (2021) 113301
Fig. 2. Chemical structures that are contained in the dyes, according to the Material Safety Data Sheet (MSDS).
0.6. Initial concentration for the black, red, yellow, cyan, green dye and
Table 1
PIW was 434 g/L, 362 g/L, 582 g/L, 580 g/L, 656 g/L and 12 g/L,
Physicochemical characterization of the printing ink wastewater used in the
respectively. The dilution ratio for the dyes at 0.3 OD was 1/100000 and
experiments. Data are presented as mean ± SD values from three separate
for the PIW was 1/80. Hence, the initial concentration in the reactor was
measurements.
4.3 mg/L and 3.6 mg/L, for the black and red dye, respectively, 5.8 mg/L
Physicochemical characteristics Value
for yellow and cyan dye, 6.6 mg/L for the green dye and 144 mg/L for
Color Black (565 nm) PIW. The dilution ratio for the dyes at 0.6 OD was 1/50000 and the
pH 7.59 ± 0.5 initial concentration in the reactor was 8.7 mg/L for the black dye, 7.2
Conductivity 17.00 ± 0.5 μS/cm
COD 21000 ± 1000 mg/L
mg/L for the red dye, 11.6 mg/L for the yellow and the cyan dye and
13.1 mg/L for the green dye. Hydrogen peroxide (H2O2 30% w/w,
Honeywell) of various concentrations (0.5, 1.0 and 2.0 g/L) was used to
determine the effect of an oxidizing agent on HC treatment. Each
experimental set was performed in duplicate. The temperature was kept
constant at 35 ±3 ◦ C by circulating water through the tank’s cooling
jacket. Total COD (Chemical oxygen demand) loads of each dye solution
were 66, 123, 85, 64, 78 mg/L for the black, red, yellow, cyan and green
dye, respectively, and the pH was 7.5 ± 0.5. The total COD of PIW was
120 mg/L and the pH 7.5 ± 0.5. The pH was not controlled in the ex
periments. Blank tests (H2O2 only, in the absence of HC) were performed
in a smaller scale (in a beaker under stirring) with 0.3 or 0.6 OD of each
dye, with constant temperature and uncontrolled pH. Different H2O2
dosages were added in the solution to investigate the ability of H2O2 to
decolorate. Furthermore, blank tests (HC in the absence of H2O2) were
performed to investigate the color removal without H2O2 in the specific
Fig. 3. Schematic representation of novel hydrodynamic cavitation pilot-scale HC reactor at the desired dye concentration at 4 bar inlet pressure with
reactor with a changeable orifice plate inside. uncontrolled pH and constant temperature.
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and 2 mm diameter, and 62 holes plates of 1 mm and 2 mm diameter) plates with 31 holes, the extent of decolorization was greater for the
and tested for their effect on the removal of the industrial-grade black plate having higher diameter of holes. Sivakumar and Pandit (2002)
dye. observed similar results for rhodamine B degradation since the decol
Fig. 5 shows the effect of orifice plate geometry at 4 bar inlet pressure orization rate was enhanced by an increase in the value of α up to 2.
on the color removal of black dye (0.3 OD, 1 g/L H2O2). Plate C (31 More information about the effect of value β of the orifice plates on color
holes, 2 mm diameter) reached higher decolorization, about 70%, while removal and a schematic representation of plates are included as sup
plates A and B with one single hole (and diameter of the holes 2 mm and plementary material (Figs. S2 and S3). These results agree with the study
1 mm) reached lower degradation 61% and 59%, respectively. Plates E of Malade and Deshannavar (2018), who examined the decolorization of
and D had almost the exact extent of decolorization 30%. Finally, the use Reactive Red 120 using hydrodynamic cavitation. Different plate ge
of plate F showed 43% color removal. Comparing firstly, the plates with ometries were tested, and the researchers observed that the process
the same diameter of the holes (i.e. 2 mm) or same α parameter, plate C performance was optimized to a specific β value. The authors justified
with 31 holes had greater degradation than plates A (with one single the existence of an optimum since an increase of flow rate, increased the
hole) or E (with 62 holes), while comparing the plates with 1 mm extent of cavitation and higher decolorization was achieved, while at the
diameter, plate D with 31 holes had lower degradation than plate B same time, with higher throat area, the velocity decreased thus resulting
(with one single hole) or F (with 62 holes). Comparing the plates with in lower performance.
the same number of holes, hole diameter makes no difference for one-
hole orifice plates, as both plates (A and B) reached almost 60% color 3.1.2. Inlet pressure
removal. For plates with 31 holes, efficiency was increased with Inlet pressure is the most important parameter determining the ef
increasing holes’ diameter, while for plates with 62 holes, the degra ficiency of pollutant degradation in an aqueous medium by hydrody
dation was reduced with increasing diameter. Finally, plate C (31 holes, namic cavitation (Lu et al., 2019). The pressure at which a medium
2 mm diameter) was considered the optimum, and all the experiments enters the HC reactor determines the intensity of the generation of
from there on were conducted using the specific plate geometry. For cavities and, in turn, the extent of degradation of the wastewater’s
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•
O H + • O H→H2 O2 (3)
Fig. 6. Color removal of black industrial-grade dye in various time intervals for •
O H + H2 O2 →HO•2 + H2 O (4)
two inlet pressures, 4 and 5 bar in the presence of 1.0 g/L H2O2. Initial OD was
set at 0.3 and plate C was used (Temperature: 35 ±3 ◦ C, pH: 7.5 ± 0.5). Data •
O H + HO•2 →H2 O + O2 (5)
are presented as mean ± SD values from three separate measurements.
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HO•2 + H2 O2 →• O H + H2 O + O2 (6)
Table 4
Color removal values for five industrial grade dyes after application of hydrodynamic cavitation (HC), hydrodynamic cavitation in the presence of various concen
trations of H2O2 (HC þ H2O2 g/L) as well as the blank testing for each application. For all experiments, the initial OD was set at 0.3, pressure at 4 bar and plate C was
used (Temperature: 35 ±3 ◦ C, pH: 7.5 ± 0.5). Data are presented as mean ± SD values from three separate measurements.
Industrial grade dye Color removal (%)
0.5 1.0 2.0 HC only 0.5 g/L H2O2 only 1.0 g/L H2O2 only 2.0 g/L H2O2 only
Black 52.9 ± 0.0 68.3 ± 4.9 59.9 ± 0.0 39.9 ± 0.8 8.0 ± 0.0 4.1 ± 2.7 14.4 ± 0.2
Red 22.7 ± 0.5 39.1 ± 7.8 22.7 ± 4.3 26.4 ± 2.0 0.0 ± 0.0 11.0 ± 2.0 0.0 ± 0.0
Yellow 40.5 ± 0.4 43.7 ± 5.2 31.1 ± 1.0 46.7 ± 0.7 5.0 ± 1.9 9.3 ± 2.1 0.0 ± 0.4
Green 47.7 ± 0.0 55.3 ± 7.3 47.0 ± 0.6 31.0 ± 4.9 13.0 ± 0.0 15.1 ± 0.9 5.0 ± 0.8
Cyan 47.6 ± 0.0 51.6 ± 4.8 43.5 ± 1.0 51.7 ± 1.1 19.0 ± 0.0 6.0 ± 0.0 2.0 ± 0.1
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reactive red 120 dye (RR120) increases with an increase in the con Table 5
centration of H2O2, reaching almost 100% decolorization at 1:60 Color removal values for five industrial grade dyes after application of hydro
(RR120: H2O2) ratio compared to only 60% reduction in color in the dynamic cavitation in the presence of 1 g/L H2O2 (HC+1 g/L H2O2) as well as
absence of H2O2 (HC only). Additionally, no improvement in the rate of the blank testing for each application. For all experiments, the initial OD was set
dye degradation was observed after an optimum concentration of H2O2. at 0.6, pressure at 4 bar and plate C was used (Temperature: 35 ±3 ◦ C, pH: 7.5 ±
0.5). Data are presented as mean ± SD values from three separate
Gore et al. (2014) recorded almost 100% decolorization of reactive or
measurements.
ange 4 dye at an optimum 1:30 M ratio of orange-G to H2O2, and no
further increment in the degradation rate was observed at a higher ratio. Industrial grade dye Color removal (%)
The present study concluded that the combined treatment method (HC Treatment Blank
+ H2O2) was 2.5 times more efficient than the HC process alone (Gore HC+1.0 g/L H2O2 HC only 1.0 g/L H2O2 only
et al., 2014). Generally, it can be deduced that the H2O2 concentration
Black 45.7 ± 4.7 23.3 ± 0.2 0.0 ± 0.0
should be optimized based on the pollutant’s molecule nature and Red 9.7 ± 4.0 11.0 ± 0.1 2.9 ± 0.0
organic loading. An excessive H2O2 amount could not only reduce the Yellow 50.9 ± 4.1 8.7 ± 0.1 16.6 ± 0.2
degradation efficiency but also negatively affect the economic feasibility Green 29.7 ± 1.1 18.0 ± 0.4 7.7 ± 0.0
of the treatment process. Table S1 in the supplementary material shows Cyan 23.2 ± 1.4 23.2 ± 0.2 7.0 ± 2.2
the performance of the process compared to similar hydrodynamic
cavitation systems for dye removal and cost estimation. However, it
more efficient. Afterwards, all industrial-grade dye solutions were
should be noted that comparison of different processes or experimental
studied at higher initial concentration (i.e., 0.6 OD) in combination with
conditions for the treatment of different industrial wastewater is purely
1.0 g/L H2O2 dosage, and the results are presented in Table 5. The data
indicative and can give misleading results.
in Table 4 (for 0.3 OD) and 5 (for 0.6 OD) show that degradation effi
ciency decreased due to higher dye initial concentration for HC+1.0 g/L
3.1.4. Initial concentration of contaminants
H2O2. The yellow dye was the only exception, and for 0.6 OD showed
Another crucial parameter that determines the efficiency of the
almost the same color removal (50.9%) as the 0.3 OD dye (43.7%). The
degradation process is the initial concentration of contaminants present
results show that, color removal reached 45% for black, 9% for red, 50%
in the aqueous solution.
for yellow, 29% for green, and 23% for cyan for 0.6 OD initial concen
Additional experiments were performed on dye solutions at 0.6 OD
tration (Table 5). Thus, higher initial concentration (0.6 OD) shows a
and applying an inlet pressure of 4 bar. Experiments were performed to
decrease of 33% for black, 75% for red, 46% for green and 55% for cyan
determine any correlation between increasing H2O2 concentration and
dye, compared to 0.3 OD, for the decolorization. This behavior (higher
color removal efficiency from 0.6 OD black dye solution. As shown in
dye initial concentration demonstrates lower degradation efficiency)
Fig. 8, HC coupled with 1.0 g/L H2O2 achieved 45.7% color removal
has been observed in other technologies such as Fenton reaction, wet
while HC coupled with 2.0 g/L H2O2 achieved almost 20% decoloriza
oxidation, and persulfate oxidation. In most cases, the radicals/pollutant
tion, for the black dye. Thus, even increase of the initial concentration
ratio is small; therefore, for a higher organic load, the in situ generated
(from 0.3 OD to 0.6 OD), HC combined with 1.0 g/L H2O2 proved to be
reactive oxygen species are the limiting factor of the process. In hy
drodynamic cavitation, an additional factor that reduces the efficiency is
the mass transfer of the pollutant inside the cavity or the cavity/bulk
solution interface.
Blank tests were also done for all dyes by treating the 0.6 OD solu
tions with 1.0 g/L H2O2 in the absence of the HC reactor and performing
HC at 4 bar in the absence of H2O2 (Table 5). H2O2 treatment alone
produced degradation rates of under 16% (specifically, 0% for black
dye, 2% for red dye, 16% for yellow dye, and around 7% for the cyan and
green dyes). Similarly, it was observed that HC only caused 23%
decolorization of the black and cyan dye solutions, and 11%, 8% and
18% of the red, yellow and green dye solutions, respectively (Table 5).
Therefore, combined HC+1.0 g/L H2O2 treatment proved more efficient
at decolorizing these dye solutions than each individual treatment
method alone.
Many researchers have studied the effect of initial pollutant con
centrations on HC efficiency (Gogate and Patil, 2015; Joshi and Gogate,
2012). Pradhan and Gogate (2010) found that p-nitrophenol removal
decreased with an increase in its initial concentration from 53.4% at 5.0
g/L to 44.8% at 10.0 g/L at 2.9 bar initial pressure when using hydro
dynamic cavitation alone. Wang et al. (2020) showed that the removal
rate of methyl orange dye, decreased with the initial concentration (5
mg/L, 10 mg/L, 15 mg/L, 20 mg/L) but increased with treatment time
(using single HC).
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C. Zampeta et al. Journal of Environmental Management 297 (2021) 113301
Fig. 9. COD removal for five industrial-grade dyes and printing ink wastewater
(PIW) after application of hydrodynamic cavitation in the presence of 1.0 g/L
H2O2 (Temperature: 35 ±3 ◦ C, pH: 7.5 ± 0.5). For all experiments, the initial Fig. 10. Color removal in various time intervals for printing ink wastewater
OD was set at 0.3 and pressure at 4 bar and plate C was used. (PIW) after application of hydrodynamic cavitation (HC), hydrodynamic cavi
tation in the presence of H2O2 1.0 g/L and only addition of H2O2 1.0 g/L. For all
experiments, the initial OD was set at 0.3 and pressure at 4 bar and plate C was
red, yellow, cyan and green dye solutions, respectively. For PIW, COD used (Temperature: 35 ±3 ◦ C, pH: 7.5 ± 0.5). Data are presented as mean ± SD
removal reached 55%. The COD of the effluent was 54 mg/L for PIW and values from three separate measurements.
0 mg/L, 76 mg/L, 63 mg/L, 21 mg/L, 17 mg/L, 54 mg/L for black, red,
yellow, cyan, green dye, respectively. real industrial effluent when HC was applied (slit Venturi as a cavitating
Many of the published studies have studied COD removal but they device, H2O2: 5 g/L, inlet pressure: 4 bar, pH: 4) while color removal was
have not achieved extremely high COD reduction. Rajoriya et al. (2018) not recorded. In another study, Rajoriya et al. (2016) studied COD
studied the efficiency of a slit Venturi HC reactor for the removal of COD reduction from an aqueous effluent by applying HC after upflow
from a textile dyeing industry effluent (TDI). COD reduction was anaerobic sludge blanket anaerobic treatment. Slit Venturi with a 3 bar
recorded as 12% using HC alone, and 38% when HC was combined with inlet pressure generated about 48% COD removal. Finally, Bis et al.
Fenton, at optimum conditions (solution volume: 6 L, pH: 6.8, pressure: (2015) tried 3 different geometries of orifice plates and reported that
5 bar, treatment time: 120 min). Li et al. (2009) reported a maximum of COD removal was around 6% for landfill leachate treatment in any case.
85.4% COD removal at optimum conditions when treating real (non-
synthetic) industrial triazophos wastewater (pH: 4, stirring time: 90 min,
and a dose of 5.0 g/L of FeSO4⋅7H2O and 75 mL/L of 30% H2O2 solu 3.4. Yield of cavitation technology
tion). Also, real wastewater from bitumen production was treated by
Boczkaj et al. (2018) using a Venturi tube (P: 7.9 atm, Q: 520 L/h, T: Cavitation yield (7) was calculated using the experimental data and
40 ◦ C, pH: 10.5, t: 360 min HC). It was found that HC+72 ml/L H2O2 and parameters obtained from the experiments described above.
HC alone achieved 20% and 13% COD reduction, respectively. ( )
L amount degraded (OD initial − OD final)
Cavitation yield OD ⋅ = PE⋅ (7)
J t
3.3. Treatment of real printing ink wastewater V
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C. Zampeta et al. Journal of Environmental Management 297 (2021) 113301
material and the results are presented in Table 6. The maximum cavi removal efficiency in many cases. However, optimization of the process
tation yield was estimated using the combination of hydrodynamic is necessary, in order to increase the efficiency of the process and to
cavitation and 1.0 g/L hydrogen peroxide (plate C, pressure: 4 bar, OD: drastically decrease the treatment time, thus reducing energy require
0.3) for all treated liquids. Cavitation yields of the combined method ment and operating costs. Optimization of pH operating range for
(HC+1.0 g/L H2O2) were higher than the blank tests (HC only) recorded wastewater is necessary, as well as of the design of the orifice plate. HC
for PIW and most dye solutions. Among all the treated liquids in the could also be combined with a post-treatment method. Simple and low-
combined method, highest yield of cavitation was estimated for black cost chemical or physical processes such electrolytes addition and
dye reaching 2.5E(-7) OD⋅L/J, while for PIW this value was one order of sedimentation could be used for complete decolorization of colorful
magnitude lower achieving 6.3E(-8) OD⋅L/J. Red, yellow, green and wastewaters.
cyan dye yields reached 1.1E(-7), 1.5E(-7), 2.0E(-7) and 1.7E(-7) OD⋅L/
J, respectively. It is worth noting that when the industrial-grade dye Credit author statement
solutions were treated with HC without the addition of hydrogen
peroxide, cavitation yields were higher for yellow and cyan, reaching Charikleia Zampeta: Methodology, Validation, Investigation,
1.6E(-7) and 1.7E(-7) OD⋅L/J, respectively. As shown in equation (7), Writing – review & editing, Writing – original draft, Visualization. Kleio
cavitation yield is proportional to color removal. Cavitation yield de Bertaki: Investigation. Irene-Eva Triantaphyllidou: Methodology, Vali
pends only on the amount of dye degraded because the fraction’s de dation, Writing – review & editing, Writing – original draft, Visualiza
nominator is always stable in all experiments. Thus, greater tion. Zacharias Frontistis: Conceptualization, Validation, Writing –
decolorization leads to a higher cavitation yield, as shown in Table 6 for original draft, Writing – review & editing, Visualization. Dimitris V.
all the dyes and PIW tested. Hence, in general, HC alone, showed lower Vayenas: Conceptualization, Validation, Writing – original draft,
cavitation yield in comparison with HC+1.0 g/L H2O2. Writing – review & editing, Supervision, Visualization.
The conclusions of the present study are in agreement with Innocenzi
et al. (2019) who demonstrated that HC (at 4 bar) combined with
0.005%v/v hydrogen peroxide showed significantly higher cavitation Declaration of competing interest
yield than HC alone (pressure: 4 bar, pH: 2, initial methyl orange con
centration: 5 mg/L). Innocenzi et al. (2019) concluded that HC should be The authors declare that they have no known competing financial
combined with other AOPs or additives to improve efficiency. Also, interests or personal relationships that could have appeared to influence
similar results were reported by Tao et al. (2016). It was concluded that the work reported in this paper.
HC coupled with an additive (i.e., CCL4 to promote the generation of
reactive species), demonstrates higher cavitation yield than HC use Acknowledgements
alone. The cavitation yields were obtained, using various hybrid ap
proaches for rhodamine B degradation. This research did not receive any specific grant from funding
agencies in the public, commercial, or not–for–profit sectors.
4. Conclusions
Appendix A. Supplementary data
A pilot-scale novel hydrodynamic cavitation (HC) reactor was
designed and constructed. The novelty of the HC reactor is based on the Supplementary data to this article can be found online at https://doi.
combination of a Venturi tube containing an orifice plate. The reactor org/10.1016/j.jenvman.2021.113301.
was tested for the treatment of industrial-grade dyes from a cardboard
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