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JOURNAL OF ENVIRONMENTAL SCIENCE AND HEALTH Part AToxic/Hazardous Substances & Environmental Engineering Vol. A38, No. 10, pp. 22412250, 2003

INDUSTRIAL WASTEWATER TREATMENT

Removal of Color and COD from a Mixture of Four Reactive Azo Dyes Using Fenton Oxidation Process
nay Sureyya Meric ,* Deniz Kaptan, and Olcay Tu
Department of Environmental Engineering, Civil Engineering Faculty, Istanbul Technical University, Maslak, Istanbul, Turkey

ABSTRACT
This study was designed to decolorize and to reduce COD content in a mixture of four reactive dyes, i.e., Remazol Black 5 (RB5), Remazol Red RB (RR), Remazol Yellow 84 (RY), Remazol Brilliant Blue (RB) using Fenton Oxidation Process (FOP). Optimum pH, temperature, and the doses of FeSO4 and H2O2 were determined. Experiments were conducted on the samples containing a total concentration of 100 mg L1 (RB RY), 200 mg L1 (RB5 RR), 300 mg L1 (RB5 RR RB RY), and 400 mg L1 (RR RB RY) dyes considering their actual application doses in dyehouses. Optimum pH was observed as 2.5 at 30 C using 400 mg L1 FeSO4 and 800 mg L1 of H2O2 resulting in more than 96% COD and 99% Pt-Co unit of color removal for the mixture of RB5 and RR. The optimum conditions determined were 4.0 pH, 50 C, and 500 mg L1 FeSO4 applying 1000 mg L1 H2O2 for the mixture of (RB5 RR RB RY). A 100 mg L1 solution of a mixture of RB and RY at equal amounts was oxidized using 200 mg L1 FeSO4 and 300 mg L1 H2O2 at 3.0 pH and 50 C. Key Words: Color; COD removal; Fentons oxidation process; Reactive dyes; Textile industry.

*Correspondence: Sureyya Meric , Department of Environmental Engineering, Civil Engineering Faculty, Istanbul Technical University, Maslak 34469, Istanbul, Turkey; Fax: 0900 212 285 6882; E-mail: smeric@ins.itu.edu.tr. 2241
DOI: 10.1081/ESE-120023371 Copyright & 2003 by Marcel Dekker, Inc. 1093-4529 (Print); 1532-4117 (Online) www.dekker.com

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INTRODUCTION Wastewaters originated from the textile industry contain various pollutants including a high content of organic matter and color problem depending on forms of dyes, surface active materials, and textile additive materials used in the process.[1] Reactive dyes having azo bounds are the most commonly applied (6070%) among more than 10,000 dyes applied in textile processing industries.[2] Discharge of azo dyes is undesirable not only for aesthetic reasons but also because many azo dyes and their breakdown products are toxic to aquatic life[3] and exhibit mutagenic/carcinogenic properties.[4] Azo dyes are resistant to biodegradation under aerobic conditions[5] whereas anaerobic color removal due to reductive NN cleavage was applied by many researchers successfully.[2,6,7] Many chemical processes have been used extensively for the treatment of textile wastewaters. Most of the studies, such as chemical precipitation,[8] adsorption by activated carbon[9] and use of some natural absorbents,[10] photocatalytic oxidation,[11] ozonation,[12,13] and Fenton oxidation process[1420] have been focused on color removal. Fenton oxidation process (FOP) has the advantages of both oxidation and coagulation processes. During FOP, the organic substances are reacted with hydrogen peroxide (H2O2) in the presence of inexpensive ferrous sulphate (FeSO4) to reduce COD content and color of wastewater.[14] FOP has been used to treat recalcitrant/toxic wastewaters.[20,21] The chemistry of FOP is explained. The reactions are given by Walling and Kato as cited in Lin and Peng.[22] COD and color removal reactions are initiated by the hydroxyl radical. H2 O2 Fe2 ! Fe3 OH  OH RH  OH ! R H2 O R Fe3 ! R Fe2 Fe2  OH ! Fe3 OH 1 2 3 4

FOP was composed of four stages, which are: pH adjustment, oxidation reaction, neutralization, and coagulation.[14] It is mentioned that for decolorization purposes of azo dyes mineralization is not necessary because the removal of color is associated with break down of the conjugated unsaturated bonds in molecules.[15] In that case the dose of H2O2 must be well dened. Kuo[14] reported that at pH lower than 3.5, H2O2 and ferrous ions are more stable resulting in a better redox system and a more eective decolorization. However, at pH values higher than 4.0, ferrous ions easily form ferric ions, which have a tendency to produce ferric hydroxo complexes. H2O2 is unstable and easily decomposes itself in the basic solutions. FOP was studied by many workers to remove color and COD from textile wastewaters. Some of these studies have focused on the dyes,[14,15,19] textile additives,[20] and textile wastewater.[1618] Kuo [14] used 1167 mg L1 of H2O2 and

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500 mg L1 of FeSO4 for 0.3 g L1 of reactive dye solution at 50 C and lower than 3.5 pH. Kang and Chang[16] used FOP for COD and color removal from articial textile wastewaters and textile secondary euents containing reactive dyes. They concluded that the optimum pH was between 3.0 and 5.0 and the determining step for COD and color removal was the oxidation rather than coagulation. Park et al.[18] applied FOP to pigment wastewaters. Optimum pH and molar Fe2/H2O2 ratio were found to be 3.0 and 0.4, respectively. Lin and Lo[17] used FOP for simulated textile dyeing wastewater containing direct and reactive dyes. Optimum values of pH, temperature, and molar FeSO4/H2O2 ratio were found to be 3.0, 30 C, and 0.09 respectively. These studies indicate the success of FOP in removing color and delineate the operating conditions. However application of FOP for the actual conditions is rare. Textile dye baths contain more than one dye stu and the mixture of dyes may respond to oxidation in a dierent way than they singly exist. The purpose of this study is to investigate the FOP applications for several dye mixtures that represent actual combinations. The investigation covered the determination of other parameters aecting the process eciency to nd out optimum values and to make comparisons with the literature values. Eect of temperature was also evaluated to assess the advantage of high temperature of spent baths.

MATERIALS AND METHODS Commonly used reactive dyes Remazol Black B(RB5), Remazol Red RB (RR), Remazol Brilliant Blue (RB), and Remazol Yellow 84 (RY) and their combinations were used in the study.

Experimental Set-Up Experimental study was designed for the optimization of COD and color removal, pH, temperature, and FeSO4 and H2O2 doses. FOP was performed by the method reported by Kuo[14] with a modication of 2 min rapid mixing (RM) at 100 rpm rst and later, 20 min slow mixing (SM) at 30 rpm followed by 30 min for settling.[23] First, the pH of the sample was lowered to desired pH value using 1 N H2SO4. FeSO4 and H2O2 were added to the 500 mL beakers containing of 100, 200, 300, and 400 mg L1 dye solutions. After rapid and slow mixing, settling period, the pH of the supernatant was readjusted using 1 N NaOH up to 7.5 and the supernatant was left to settle for 2 h. During mixing, reactors were kept at constant temperature. Experiments were conducted on the dye solutions at 30, 40, 50, and 60 C temperatures changing FeSO4 and H2O2 molar ratio ranging from 0.05 to 1.25. pH was changed between 2.5 and 4.0. The study was designed in 5 stages. In the rst stage H2O2, temperature, pH, rapid and slow mixing were kept constant to determine optimum FeSO4 concentration yielding maximum color and COD removals. In the second stage, using optimum FeSO4 concentration and the same oxidation conditions, optimum H2O2

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concentration was investigated. By considering the optimum doses of rst and second stages, pH, and temperature were investigated in the third, fourth stages, respectively. The eect of the mixture time was also studied.

Analytical Measurements COD was measured according to Standard Methods.[24] Absorbance measurements were made using Pharmacia LKB-Novaspe II model spectrophotometer. HACH-Dr-B model spectrophotometer was used for the color measurements in APHA Pt-Co unit. The euent was ltered by 0.45 mm Millipore membrane lter for measuring COD, color, and absorbance at 436, 525, and 620 nm wavelengths considering German Water Discharge Standards.[25] FeSO4 solution was prepared daily and H2O2 (30%) solution was of analytical grade. Reactive dyes were obtained from a dyestu company. The solution of each dye was hydrolyzed at pH higher than 11.5 and at 80 C temperature for at least 4 h according to literature.[5] H2O2 was destroyed before COD measurements by increasing the pH over 9 and aerating the sample for 30 min.

RESULTS AND DISCUSSION COD equivalents of the dyes were determined as 0.75 mg COD mg1 RB5, 2.2 mg COD mg1 RR, 1.5 mg COD mg1 RB, and 1.5 mg COD mg1 RY, respectively. The matrix illustration of dye mixtures including COD contents of each one is seen in Table 1. The concentrations of the dyes were chosen taking into account their actual uses in the textile industry. Experimental results of FOP for dening optimum conditions are given below. According to the results of FeSO4 optimization as seen in Table 2, maximum COD removal was obtained as (88%) using 300 mg L1 FeSO4 and 600 mg L1 H2O2. However the color removal was relatively low (>91%). The absorbance measurements showed that the limits could not be provided at 436 and 525 wavelengths. Thus the concentration of H2O2 was increased up to 800 mg L1 yielding (90%) COD and (97%) color removal (Table 3). In this case, the absorbances were lowered than the limits starting from the 300 mg L1 of FeSO4. pH, temperature, and slow mixing were kept at 3.0 and 40 C, respectively.

Table 1.

The mixtures of the reactive dyes and their total COD contents. Concentration of the dyes used (mg L1) COD of dye mixture (mg L1) 295 445 740 150

RB5 Run Run Run Run 1 2 3 4 100 100

RR 100 100 200

RB 50 100 50

RY 50 100 50

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Table 2. The relation between FeSO4 concentration and color and COD removals for the mixture of RB5 and RR at 40 C, 3.0 pH, 2 min rapid mixing, 20 min slow mixing using 600 mg L1 of H2O2. FeSO4 (mg L1) 100 150 200 250 300 Absorbance 436 nm 0.31 0.16 0.10 0.12 0.20 525 nm 0.230 0.150 0.066 0.068 0.067 620 nm 0.082 0.073 0.012 0.015 0.016 Color Pt-Co 800 460 260 350 410 Pt-Co removal (%) 85 92 94 92 93 COD (mg L1) 64 60 55 42 36 COD removal (%) 78 80 81 86 88

Table 3. The relation between FeSO4 concentration and color and COD removals for the mixture of RB5 and RR at 40 C, 3.0 pH, 2 min rapid mixing, 20 min slow mixing using 800 mg L1 of H2O2. FeSO4 (mg L1) 100 200 300 400 Absorbance 436 nm 0.290 0.140 0.065 0.003 525 nm 0.240 0.079 0.021 0.002 620 nm 0.088 0.027 0.009 0.001 Color Pt-Co 700 400 150 10 Pt-Co removal (%) 87 93 97 >99 COD (mg L1) 69 46 33 15 COD removal (%) 77 84 90 95

For the optimization of H2O2 concentration, 300 mg L1 of FeSO4 was chosen. As depicted in Table 4, COD removal eciency increased by increasing H2O2 concentration from 600 mg L1 (88%) to 900 mg L1 (92%). Color removal and absorbance measurements conrmed the optimum H2O2 concentration as 800 mg L1 resulting in 97% color and 90% COD removal. To determine the optimum pH, pH was changed between 2.5 and 4.0 as shown in Table 5. Although more than 99% color removal was obtained at all pH values, the maximum COD removal (96%) was proved at 2.5 pH. The absorbances were also measured lower than the limits at each pH. As seen in Table 6, optimum temperature was found as 30 C at which 96% COD and 99% color removal were obtained. Table 7 presents the results of optimization of slow mixing time. Color was removed higher than 99% for all mixing times. Maximum COD removal (97%) was obtained at 10th min. Optimum conditions determined for 100 mg L1 of RB5, 100 mg L1 RR, and 200 mg L1 of their mixture are summarized in Table 8. Upon the data given in Table 8, molar ratio between FeSO4 and H2O2 was determined as 0.055 for RB5, 0.11 for RR, and 0.11 for their mixture. Although color removal was obtained (higher than 99%) at almost all conditions for each dye and their mixture. COD removal varied

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Table 4. The relation between H2O2 concentration and color and COD removals for the mixture of RB5 and RR at 40 C, 3.0 pH, 2 min rapid mixing, 20 min slow mixing using 300 mg L1 of FeSO4. H2O2 (mg L1) 600 700 800 900 Absorbance 436 nm 0.200 0.140 0.065 0.012 525 nm 0.067 0.040 0.021 0.004 620 nm 0.016 0.011 0.009 0.002 Color Pt-Co 410 300 150 30 Pt-Co removal (%) 93 95 97 99 COD (mg L1) 36 32 30 24 COD removal (%) 88 89 90 92

Table 5. The relation between pH and color and COD removals for the mixture of RB5 and RR at 40 C, 2 min rapid mixing, 20 min slow mixing using 400 mg L1 of FeSO4 and 800 mg L1 of H2O2. Absorbance pH 2.5 3.0 3.5 4.0 436 nm 0.002 0.003 0.006 0.003 525 nm 0.001 0.002 0.004 0.001 620 nm 0.001 0.001 0.003 0.001 Color Pt-Co <10 <10 <10 <10 Pt-Co removal (%) >99 >99 >99 >99 COD (mg L1) 10 15 17 20 COD removal (%) 96 94 93 92

Table 6. The relation between temperature and color and COD removals for the mixture of RB5 and RR at 3.0 pH, 2 min rapid mixing, 20 min slow mixing using 400 mg L1 of FeSO4 and 800 mg L1 of H2O2. Absorbance T( C) 30 40 50 60 436 nm 0.002 0.003 0.003 0.002 525 nm 0.001 0.002 0.002 0.001 620 nm 0.001 0.001 0.001 0.001 Color Pt-Co <10 <10 <10 <10 Pt-Co removal (%) >99 >99 >99 >99 COD (mg L1) 10 15 19 21 COD removal (%) 96 94 93 92

between 7086% for RB5, 8595% for RR, and 8096% for their mixture. Lower COD removal eciency of RB5 indicated that its oxidation was more dicult than RR. In the case of the oxidation of their mixture, it was necessary to increase the doses of FeSO4 and H2O2 more than 2 fold. However, increasing ratio of the H2O2 dose (1000 mg L1 for both RB5 and RR) was lower than their individual 200 mg L1 uses.[23] Optimum temperature and pH values of their mixture (30 C,

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Table 7. The relation between mixing time and color and COD removals for the mixture of RB5 and RR at 40 C, 3.0 pH, 2 min rapid mixing, 20 min slow mixing time (SM) using 400 mg L1 of FeSO4 and 800 mg L1 of H2O2. Absorbance SM (min) 10 15 20 30 436 nm 0.002 0.001 0.003 0.001 525 nm 0.001 0.001 0.002 0.001 620 nm 0.001 0.001 0.001 0.001 Color Pt-Co <10 <10 <10 <10 Pt-Co removal (%) >99 >99 >99 >99 COD (mg L1) 10 8 15 18 COD removal (%) 97 96 94 93

Table 8.

Optimum removal conditions for RB5, RR, and their mixture using FOP process. RB5 RR 100 95 >99 50 3.5 150 300 0.11 RR 200 94 >99 50 3.5 250 1,000 0.055 Mixture of RB5 RR 200 96 >99 30 2.5 400 800 0.11

Dye concentration (mg L1) COD removal (%) Color removal (%) T ( C) pH FeSO4 (mg L1) H2O2 (mg L1) Molar ratio [FeSO4/H2O2]

100 7086 (86.4)* >99 40 3.0 (3.5)* 100 400 0.055

*Maximum eciency obtained at 3.5 pH.

Table 9. Composition Dye concentration (mg L ) COD removal (%) Color removal (%) T( C) pH FeSO4 (mg L1) H2O2 (mg L1) FeSO4/H2O2 molar ratio
1

FO process results for the mixture of dyes. Run 2 300 93 >99 50 4 500 1,000 0.11 Run 3 400 94 (96)* >99 30 3 (4)* 600 1,000 0.13 Run 4 100 93 91 50 3 200 300 0.15

*Maximum eciency obtained at 4 pH.

2.5 pH) were quite dierent from each dye (40 C and 3.0 pH for RB5, 50 C and 3.5 pH for RR). Considering the methodology explained for Run 1, Runs 24 were performed in the same context. The results of Run 2, 3, and 4 are shown together in Table 9.

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As seen from the results, the presence of RB and RY in the mixture of RB5 and RR (Run 2) changed the optimum oxidation conditions of RB5, RR, and their mixture as depicted in Table 8. The increase of the dose of FeSO4 was higher for Run 3 with respect to Run 2. To obtain high COD and color removals (>90%) the doses of FeSO4 and H2O2 had to be increased up to 500600 mg L1 and 1000 mg L1, respectively. However, that increase did not change the molar ratio of Run 2 and Run 3, although to treat the mixture solution of RB and RY (Run 4) seemed to be rather dicult with respect to the Run 1, 2, and 3. It can be concluded from this study that 2 min rapid mixing phase served as accelerator for formation and the consuming up the radicals in the oxidation reactions resulting in the shortened total reaction time and yielding higher color and COD removals. It was observed that increasing the dye concentration improved the oc structure in the coagulation phase. Increasing the concentration of FeSO4 did not improve COD removal eciency signicantly, whereas the change of pH aected system performance more eectively. Moreover, absorbance measurements were helpful for dening the optimum process conditions. The purpose of the study was to comparatively assess the oxidation characteristics of a mixture of dyes via FOP. Results of this study indicated the dierences between the combination of dyes. H2O2 requirement seems to be related to initial COD of the sample. The optimum pH range of 2.54.0 corresponds to the pH range given for FOP.[14] FeSO4/H2O2 ratios found were also in accordance with the literature value of 0.09.[17]

CONCLUSIONS The removal of color and COD in the mixture of RB5, RR, RB, RY azo dyes was studied by using FOP. A systematic approach with four stages, which are the determination of concentrations of FeSO4 and H2O2, pH, temperature was applied to the dye mixtures in the manner of a matrix use. The eect of mixing time on optimum conditions of FOP was also investigated. The results obtained from this study explain the Fenton oxidation pattern of reactive dyes in the case of the mixed use. FOP performed eectively to remove color and COD at high eciency (>90%) of the dye mixtures. It seemed that the dyes used in the mixtures were oxidized in the sequence RR, RB5, than RB and RY since their addition to the mixtures (Run 2 and 3) reected dierent optimum oxidation conditions. The temperature did not aect the color removal signicantly. 30 C may be accepted as an optimum for the cases studied. Increasing total dye concentration in the solution required increasing the use of FeSO4 and H2O2 to remove color and COD content. The optimum pH changed between 2.54.0 indicating that the addition of RB and RY caused a shift in pH from 3.0 to 4.0. Whereas the temperature for the mixtures varied between 30 C and 50 C. More than changing FeSO4 concentration, increasing the concentration of H2O2 and the change of pH aected system performance signicantly.

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ACKNOWLEDGMENTS This work was partially supported by a grant from the ITU Research and Development Center (Project No. 1989) and Scientic Research Council of _C Turkey (I TAG-C 035). The authors gratefully thank Huseyin Selcuk for his helps.

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17. Lin, S.H.; Lo, C.C. Fenton process for treatment of desizing wastewater. Water Res. 1997, 31, 20502056. 18. Park, T.J.; Lee, K.H.; Jung, E.J.; Kim, C.W. Removal of refractory organics and color in pigment wastewater with Fenton Oxidation. Water Sci. Technol. 1999, 39, 189192. 19. Arslan, I.; Balcioglu, A. Degradation of Remazol Black B Dye and its simulated dyebath wastewater by advanced oxidation processess in heterogenous and homogeneous media. Color Technol. 2001, 117, 3842. 20. Kang, S-F.; Liao, C-H.; Chen, M-C. Pre-oxidation and coagulation of textile wastewater by the Fenton Process. Chemosphere 2002, 46, 923928. 21. Gulyas, H. Processes for the removal of recalcitrant organics from industrial wastewaters. Water Sci. Technol. 1997, 36 (23), 916. 22. Lin, S.H.; Peng, C.F. A continuous fentons process for treatment of textile wastewater. Environ. Technol. 1995, 16, 693699. 23. Kaptan, D. Toxicity reduction in textile industry wastewater. M.Sc. Thesis, 2002; Istanbul Technical University, Institute of Science and Technology, Istanbul, Turkey (in Turkish). 24. APHA-AWWA-WPCF. Standard Methods for the Examination of Water and Wastewater; 20th Ed.; Washington DC, USA, 1998. 25. Gahr, F.; Hermanutz, F.; Oppermann, W. OzonationAn important technique to comply with new German Laws for textile wastewater. Water Sci. Technol. 1994, 30, 255263.

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