Treatment of Distillery Industrial Wastewater Using Ozone Assisted Fenton’s Process: Color and Chemical Oxygen Demand Removal with Electrical Energy per Order Evaluation

Asaithambi, Perumal; Busier Yesuf, Mamuye; Kebede Debela, Seifu; Govindarajan, Rajendran; Hariharan, N. M.; Alemayehu, Esayas

doi:https://doi.org/10.1155/2022/5006911

International Journal of Chemical Engineering

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Abstract Introduction Materials and Methods Results and Discussion Conclusion Data Availability Conflicts of Interest References Copyright Related Articles

Research Article | Open Access

Volume 2022 | Article ID 5006911 | https://doi.org/10.1155/2022/5006911

Treatment of Distillery Industrial Wastewater Using Ozone Assisted Fenton’s Process: Color and Chemical Oxygen Demand Removal with Electrical Energy per Order Evaluation

Perumal Asaithambi,¹Mamuye Busier Yesuf,¹Seifu Kebede Debela,¹Rajendran Govindarajan,²N. M. Hariharan,³and Esayas Alemayehu^1,4

Academic Editor: Sébastien Déon

Received12 Feb 2022

Revised18 Mar 2022

Accepted29 Mar 2022

Published20 Apr 2022

Abstract

Ozonation is one of the most effective and efficient advanced oxidation processes (AOPs) and has shown great potential in the treatment of industrial effluent and wastewater. In the present work, the ozone-Fenton process for % COD and color removal together with electrical energy per order (EE/O) determination for distillery industrial wastewater (DIW) was established. The process was developed by combining the ozone (O₃) with the Fenton (Fe²⁺/H₂O₂) process. The ozone-Fenton (O₃/Fe²⁺/H₂O₂) was compared with other treatment processes such as O₃, Fe²⁺, H₂O₂, O₃/Fe²⁺, O₃/H₂O₂, and Fe²⁺/H₂O₂ for EE/O together with % COD and color removal efficiency for DIW. The removal of color at 100% and chemical oxygen demand (COD) of 96.875% were achieved with a minimum of EE/O of 0.5315 kWh/m³ using the O₃/Fe²⁺/H₂O₂ process by operating at optimum conditions. The % COD and color values obtained using O₃/Fe²⁺/H₂O₂ were significantly higher than those obtained using O₃, Fe²⁺, H₂O₂, O₃/Fe²⁺, O₃/H₂O₂, and Fe²⁺/H₂O₂ processes. The % color, % COD removal, and its associated EE/O were evaluated by varying Fe²⁺, H₂O₂, O₃ inlet and COD concentration, and initial wastewater pH using the O₃/Fe²⁺/H₂O₂ process. The synergy effect of the O₃ and Fe²⁺/H₂O₂ processes was evaluated and reported. Our experimental findings suggest that combining O₃ with the Fe²⁺/H₂O₂ process could effectively treat industrial effluent and wastewater.

1. Introduction

Nowadays, the ozonation (O₃) process is commonly used to treat water, wastewater, and industrial effluents in a variety of applications, including disinfection of swimming pool [1], drinking [2], domestic [3], distilleries [4, 5], fermentation [6], dyeing [7], slaughterhouse [8], laundry [9], municipal [10], pharmaceutical [11], synthetic textile [12], RB 5 dye [13], laboratory [14], and petrochemical [15]. The use of O₃ in wastewater treatment to disinfect, deodorize, decolorize, and oxidize is becoming essential, particularly when a high degree of treatment is required [6, 16]. It has high efficiency of pollutant removal, an absence of secondary contamination, and a short residence time for wastewater treatment. In comparison to other methods of wastewater treatment such as physical, chemical, biological process, electrochemical [17, 18], and advanced oxidation processes (AOPs) [18, 19], the O₃ process has advantages such as high oxidizing ability, nonselective simple reaction conditions, without the need for high temperature or pressure [20], etc.

Ozone has a high oxidation potential and produces the hydroxyl radical (^•OH), a highly reactive oxidative species [21, 22]. While O₃ has high oxidizing power, its conversion to ^•OH is inefficient, and thus O₃ alone has a lower capacity for pollutant removal than ^•OH [23]. Consequently, in recent years, new O₃ hybrid processes based on AOPs and electrochemical processes have been developed, including catalytic, nanocatalyzed, photocatalytic, and sonolytic ozonation, O₃/UV, O₃/H₂O₂, O₃/Fenton, O₃/electrochemical, and O₃/UV/H₂O₂ [21, 24]. The addition of Fe²⁺ and H₂O₂ to O₃, referred to as the O₃/Fe²⁺/H₂O₂ process [25], improves the decolorization/degradation/mineralization of organic/inorganic matter present in effluent and wastewater [26, 27]. The O₃/Fe²⁺/H₂O₂ process produced additional ^•OH radicals via the reaction of O₃ with Fe²⁺/H₂O₂, and the reactions are described elsewhere [28, 29].

Owing to the synergic effect, the combination of O₃ with Fe²⁺/H₂O₂ reagent exhibits a high oxidation rate. The O₃/Fe²⁺/H₂O₂ process produces excessive ^•OH via the reaction of O₃ and Fe²⁺/H₂O₂, resulting in increased pollutant removal at a reduced treatment time. The O₃/Fe²⁺/H₂O₂ has been used to treat water present in various types of wastewater, such as urban [30] and landfill leachate [31]. A comparison showed that O₃ and Fe²⁺/H₂O₂ processes were both less effective than the O₃/Fe²⁺/H₂O₂ combination [32].

Feng et al. examined the degradation of spent resin using the O₃–Fe²⁺/H₂O₂ and Fe²⁺/H₂O₂ processes and concluded that both processes run according to first-order kinetic equations, and the O₃–Fe²⁺/H₂O₂ process had the maximum removal competence and cost savings [32]. Li et al. compared the Fe²⁺/H₂O₂ and O₃/Fe²⁺/H₂O₂ processes for amoxicillin degradation. The COD–65% removal rate was achieved in the O₃–Fe²⁺/H₂O₂ process as opposed to the Fe²⁺/H₂O₂ process. The synergistic effects worked in harmony with each other, thereby giving the O₃/Fe²⁺/H₂O₂ process the edge [33]. Goi et al. evaluated individual processes such as Fe²⁺/H₂O₂, O₃, and the combination of these treatment processes using leachate waste. They discovered that the coupled Fe²⁺/H₂O₂ and O₃ processes eliminated the most COD (77 %) as compared to other approaches [34].

Substantial research has concentrated on the elimination of pollutants from simulated wastewater using O₃ and AOPs, with only a few studies using real industrial effluent and wastewater. Furthermore, prior research has concentrated on the efficiency of hybrid O₃-based AOPs in terms of % COD and color removal (%) but has not put an emphasis on pollutant elimination together with electrical energy per order (EE/O). It was crucial to establish the EE/O of O₃-based AOPs to determine the process’s operating costs and feasibility. As a result, the current research concentrated on the determination of EE/O while removing color and COD from DIW utilizing the O₃ and Fe²⁺/H₂O₂ coupled AOPs process.

The primary goal of this study is to assess the efficiency of coupled O₃ and Fe²⁺/H₂O₂ based AOPs in terms of % COD and color removal, as well as the determination of EE/O in distillery industrial wastewater (DIW). This study investigated the influence of various operating conditions on the O₃/Fe²⁺/H₂O₂ process such as Fe²⁺ (5–30 mM) and H₂O₂ concentration (20–140 mM), initial pH of wastewater (1–11), COD (800–4800 ppm), and O₃ inlet concentration (0.80–4 g/hr). The synergy between the combined O₃ and Fe²⁺/H₂O₂ processes was investigated and recorded.

2. Materials and Methods

2.1. Wastewater Collection and Characterization

Distillery industrial wastewater was collected from distilleries in Erode, Tamil Nadu, India. The wastewater had the following characteristics: dark brown color, burn sugar odor, pH: 4.1–4.3, chemical oxygen demand (COD) of 80,000–90,000 mg/L, biochemical oxygen demand (BOD) of 7000–8000 mg/L, total dissolved solids (TDS) of 5550–5750 mg/L, and total suspended solids (TSS) of 15.44 g/L.

The chemicals used in the experiments were H₂O₂–50% (w/w), FeSO₄.7H₂O, NaOH, H₂SO₄, Na₂S₂O₃, KI, K₂Cr₂O₇, etc. The analytical reagent (AR) grade chemicals were purchased from Merck, India. They were used as received without any purification.

2.2. Experimental Setup

The experimental setup for the O₃/Fe²⁺/H₂O₂ process is depicted in Figure 1. The O₃ was generated with the aid of an ozone generator (Ozonetek Limited, Chennai). The air was pumped at a rate of 20 liters per minute (LPM) and generated up to 4 g/hr of O₃. The generated O₃ is directed into the reactor, which has a capacity of 500 mL. The O₃ was purged via a diffuser at the reactor’s bottom. The residual O₃ in the gas stream leaving the reactor was destroyed by the 2–5% KI solution. The DIW was adjusted to the necessary pH and COD concentrations and was loaded into the reactor along with the measured amount of Fe²⁺ and H₂O₂.

The concentration of O₃ was determined using the iodometric titration process. After the process, the samples were taken from the reactor and immediately added to Na₂S₂O₃ to stop the reaction. After centrifuging for 15 minutes at 15000 rpm, the supernatant was collected and analyzed for color using a UV/Vis–Spectrophotometer (TR300 Spectroquant®) and for COD using the principle of the closed reflux method (TR320, Spectroquant®).

2.3. Analysis

2.3.1. COD Removal (%)

The COD removal efficiency was measured using the following equation:where COD_Ini and COD_Fin are the chemical oxygen demand (mg/L) values of DIW before and after the treatment process.

2.3.2. Color Removal (%)

The color removal efficiency was calculated using the following equation:where Abs_Ini and Abs_Fin are the absorbances of the before and after treatment process of DIW.

2.3.3. Electrical Energy per Order (EE/O)

Electrical energy per order has emerged as an additional and effective way to determine the suitability of wastewater treatment, and it must be economical for both individual and combined processes [35].

The equation proposed for the determination of EE/O for COD removal is as follows:where P is the power (kW) for O₃, t is the treatment time (min), V is the volume of the reactor (L), k is the pseudo-first-order rate constant (min⁻¹) for the deterioration of the pollutant concentration.

Combining equations (3) and (4), EE/O becomes

2.3.4. Synergistic Effect (SE)

The synergy effects (SE) of the O₃/Fe²⁺/H₂O₂ process can be determined from the COD and/or color removal rate constants of the coupled and standalone processes using the following equation (6) [36]:where, , , are the rate constants of the O₃/Fe²⁺/H₂O₂, O_3, and Fe²⁺/H₂O₂ system, respectively.

A SE value ≥ 1 indicates that the coupled process surpasses the sum of the individuals, instead of SE ≤ 1 means that the coupled process produces a negative effect in combining the individuals.

3. Results and Discussion

3.1. Process Comparisons

The individuals such as Fe²⁺, H₂O₂, O₃, and hybrid processes such as Fe²⁺/H₂O₂, O₃/Fe²⁺, O₃/H₂O₂, and O₃/Fe²⁺/H₂O₂ was carried out under the following operating conditions: COD—1600 mg/L, pH—6, Fe²⁺—20 mM, H₂O₂—100 mM, and O₃ flow rate and concentration of 20 LPM and 4 g/hr, respectively. The efficiency of these processes was compared in terms of % COD and color reduction, accompanied by an estimate of EE/O for DIW, and the findings are depicted in Figures 2(a) and 2(b). As represented in Figure 2(a), the single Fe²⁺, H₂O₂, and O₃ methods were ineffective at removing color and COD. The Fe²⁺/H₂O₂ process removed % COD and color at a moderate rate. The % COD and color removed by combining O₃ with Fe²⁺ and H₂O₂ processes such as O₃/Fe²⁺, O₃/H₂O₂, and O₃/Fe²⁺/H₂O₂ were approximately 46.87%, 68.75%, and 96.87%, and 57.43%, 79.74%, and 100%, respectively. As predicted, the hybrid O₃/Fe²⁺/H₂O₂ process is more efficient at removing COD and color than the O₃/Fe²⁺ and O₃/H₂O₂ treatment processes. The abovementioned results suggested that adding Fe²⁺ and H₂O₂ to the O₃ process significantly increases COD and color removal. Perhaps this is due to the influence of concurrent pathways capable of producing plenteous ^•OH radicals for COD and color removal from DIW [37, 38].

(a)

(b)

The suitability of the O₃/Fe²⁺/H₂O₂ process for wastewater treatment is primarily determined by the EE/O, which relies on COD removal using equation (3). A minimum of 0.2 kWh/m³order¹ of EE/O was needed to remove COD and color from DIW using the O₃/Fe²⁺/H₂O₂ process. In comparison to the O₃/Fe²⁺/H₂O₂ process, the other single and combined processes such as O₃ and O₃/Fe²⁺, O₃/H₂O₂ required a high amount of EE/O to remove COD and color.

3.2. Various Operating Parameters

Experimental operating parameters including the Fe²⁺, H₂O₂, COD, and O₃ inlet concentration, and initial wastewater pH [39, 40], and so on, are found to have a major effect on the efficacy of the combined O₃/Fe²⁺/H₂O₂ process in terms of COD, color removal, and EE/O of DIW.

3.2.1. Effect of Fe²⁺

The concentration of Fe²⁺ and H₂O₂ is an important operating parameter, affecting the efficiency of pollutant removal through the O₃/Fe²⁺/H₂O₂ process and preventing the excessive use of Fe²⁺ and H₂O₂ [29, 41]. Figure 3 illustrates the significance of the amount of Fe²⁺ on the % COD reduction and EE/O in the O₃/Fe²⁺/H₂O₂ method. As illustrated in Figure 3, around 96.87% COD removal and 0.5315 kWhr/m³ EE/O were observed in the O₃/Fe²⁺/H₂O₂ process at a Fe²⁺ concentration of 20 mM in comparison to other Fe²⁺ concentrations. The combination of Fe²⁺ and H₂O₂ increases the development of ^•OH and thus the oxidation efficiency. This may be because the increased Fe²⁺ concentration facilitated the formation of ^•OH radicals, thereby accelerating DIW degradation [41]. As Fe²⁺ concentrations exceeded 20 mM, the excess Fe²⁺ absorbed ^•OH radicals, resulting in a small decline in % COD reduction and a rise in EE/O of DIW [40]. Thus, the optimal Fe²⁺ concentration was estimated to be 20 mM.

3.2.2. Effect of H₂O₂

The influence of varying the H₂O₂ concentration from 20 to 140 mM on the effectiveness of the O₃/Fe²⁺/H₂O₂ process in terms of % COD reduction and EE/O for DIW was studied, with the findings shown in Figure 4. The H₂O₂ dose added had a major effect on the studied process. According to Figure 4, the % COD removal increases from 40.63 to 96.87%, and the EE/O decreases from 3.53 to 0.53 kWhr/m³ as the initial H₂O₂ dose increases to a certain point, reaching a maximum at an initial H₂O₂ dose of about 100 mM, resulting in a substantial increase of process performance. At high concentrations of H₂O₂, it functions as an efficient ^•OH scavenger [41, 42], depending on the pollutant in concern. The observation is consistent with the following empirical equation (7):

While promotes radical chain reactions and is an effective oxidant in its own right, it has a much lower oxidation potential than ^•OH. Thus, when H₂O₂ concentrations are too high, the treatment efficiency is reduced, and its concentration must be tailored for each form of wastewater. The increase in H₂O₂ dosage increases the number of active sites on the surface, facilitating the decomposition of O₃ molecules into additional ^•OH. Thus, the O₃/Fe²⁺/H₂O₂ process demonstrates an improvement in COD efficiency as the H₂O₂ dose is increased.

3.2.3. Effect of Wastewater pH

The pH of wastewater at its initial state is critical because it affects the reaction of organic/inorganic compounds with the O₃/Fe²⁺/H₂O₂ system [25]. Figure 5 shows the results of an investigation into the impact of the initial values of pH on the % COD reduction and EE/O in the O₃/Fe²⁺/H₂O₂ process for the DIW. As shown in Figure 5, with the O₃/Fe²⁺/H₂O₂ process, the highest % COD removal efficiency and the lowest EE/O occurred at an initial pH of 6. As the pH increased up to 6, COD removal increased and EE/O decreased. Lower values of pH reveal the H⁺ ion’s scavenging effect on ^•OH, the creation of by reaction between H₂O₂ and H⁺, resulting in increased H₂O₂ stability and decreased % COD removal efficiency. The % COD reduction improved as the pH increased from 1 to 6, owing to the increased formation of ^•OH (a more powerful oxidant than O₃) via the hydroxylation reaction with O₃.

Furthermore, raising the wastewater pH to 6 in the combined O₃/Fe²⁺/H₂O₂ process resulted in coagulation, which increases contaminants through the complexation reaction induced by the transformation of Fe²⁺ and Fe³⁺ to Fe(OH)_n-type structures [25]. When the pH was greater than 6, COD removal decreased marginally with increasing pH. It is deduced that COD removal exists as a eupterotid that is energetic and easily reacts with the hydroxyl ion in acidic conditions, but it acts as a stable molecule in basic conditions, resulting in a decrease in % COD reduction and an increase in EE/O as the pH increases.

3.2.4. Effect of COD Concentration

The initial pollutant content is critical in the O₃/Fe²⁺/H₂O₂ process wastewater treatment process [43, 44]. The increased initial COD concentration from 800 to 4800 mg/L, then decreased the % COD elimination from 100 to 45.83%, with a rise in the EE/O from 0.07 to 3 kWh/m³order¹ for DIW using the O₃/Fe²⁺/H₂O₂ process, as presented in Figure 6. Since, raising the initial COD content promoted the creation of intermediate products that compete with the O₃-consuming pollutant, thus decreasing % COD removal performance, and increase of EE/O for DIW [45].

3.2.5. Effect of O₃ Inlet Concentration

It is critical to select the optimal O₃ inlet concentration for pollutant removal from wastewater when using the O₃/Fe²⁺/H₂O₂ process [40, 46]. The effect of O₃ inlet concentration on the % COD removal efficiency and EE/O with the O₃/Fe²⁺/H₂O₂ process was explored by bubbling ozone into the DIW solution at different gas concentrations ranging from 0.8 to 4 g/h. As shown in Figure 7, the % COD reduction improved from 52.18 to 96.87% and the EE/O reduced from 2.49 to 0.535 kWh/m³ order¹ as the O₃/Fe²⁺/H₂O₂ system’s O₃ concentration increased from 0.8 to 4 g/hr. This can be explained by the fact that the two key parameters, O₃ concentration and O₃–liquid mass transfer resistance, have a massive effect on the mass transfer rate of O₃ [40, 46]. With a higher O₃ concentration, the driving factor for O₃ mass transfer is increased, allowing the DIW solution to absorb more O₃. As a consequence, the excess O₃ in the solution interacted with radical initiators (Fe²⁺, H₂O₂, ^•OH, etc.) to produce more ^•OH, which eventually improves COD and color removal efficiency while lowering EE/O. Zhao et al. [46] reported similar results for the removal of Ni-EDTA using O₃-based oxidation processes.

3.3. Synergy Effect

The O₃ and Fe²⁺/H₂O₂ processes were carried out under the best experimental conditions to determine the synergy among each process for the removal of % color and % COD from DIW. The experimental findings confirmed a synergy index among O₃ and Fe²⁺/H₂O₂ processes for COD removal of DIW. Thus, as opposed to other processes (O₃ and Fe²⁺/H₂O₂), the O₃/Fe²⁺/H₂O₂ process greatly improves COD and color removal. Equation (6) was used to determine the synergy index of the O₃ and Fe²⁺/H₂O₂ processes [36]. The synergy index was 21.50%, suggesting that the effectiveness in terms % color and % COD removal was sufficiently greater for the combined process than for the individual O₃ and Fe²⁺/H₂O₂ processes. The reported synergy index is due to the fact that combining O₃ and Fe²⁺/H₂O₂ provides a larger volume of ^•OH, which enhances the rate of % color and COD removal from DIW. Thus, the coupled O₃ and Fe²⁺/H₂O₂ processes offer an alternative and novel approach for industrial wastewater treatment.

4. Conclusion

The developed O₃/Fe²⁺/H₂O₂ process is compared to O₃, Fe²⁺, H₂O₂, O₃/Fe²⁺, and O₃/H₂O₂, Fe²⁺/H₂O₂ processes, and the outcomes indicate that the O₃/Fe²⁺/H₂O₂ process is a promising method for achieving high % color and % COD removal efficiencies while consuming a minimal amount of EE/O from DIW. The findings suggest that to ensure an effective treatment process, operating parameters such as Fe²⁺, H₂O₂, COD, and O₃ inlet concentration, and initial wastewater pH should be considered. A synergy effect was calculated to exist between the O₃ and Fe²⁺/H₂O₂ processes at 21.50 percent. The O₃/Fe²⁺/H₂O₂ method was found to be capable of eliminating pollutants from a range of industrial effluents and wastewater.

Data Availability

The datasets analyzed during the study are available from the corresponding author on request.

Conflicts of Interest

The authors acknowledge that they have no conflicts of interest.

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Copyright © 2022 Perumal Asaithambi et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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International Journal of Chemical Engineering

Treatment of Distillery Industrial Wastewater Using Ozone Assisted Fenton’s Process: Color and Chemical Oxygen Demand Removal with Electrical Energy per Order Evaluation

Abstract

1. Introduction

2. Materials and Methods

2.1. Wastewater Collection and Characterization

2.2. Experimental Setup

2.3. Analysis

2.3.1. COD Removal (%)

2.3.2. Color Removal (%)

2.3.3. Electrical Energy per Order (EE/O)

2.3.4. Synergistic Effect (SE)

3. Results and Discussion

3.1. Process Comparisons

3.2. Various Operating Parameters

3.2.1. Effect of Fe2+

3.2.2. Effect of H2O2

3.2.3. Effect of Wastewater pH

3.2.4. Effect of COD Concentration

3.2.5. Effect of O3 Inlet Concentration

3.3. Synergy Effect

4. Conclusion

Data Availability

Conflicts of Interest

References

Copyright

3.2.1. Effect of Fe²⁺

3.2.2. Effect of H₂O₂

3.2.5. Effect of O₃ Inlet Concentration