A parametric study on the decolorization and mineralization of C.I. Reactive Red 141 in water by heterogeneous Fenton-like oxidation over FeZSM-5 zeolite
© Yaman and Gündüz; licensee BioMed Central. 2015
Received: 18 April 2014
Accepted: 20 January 2015
Published: 31 January 2015
In this study, the heterogeneous Fenton-like degradation of Reactive Red 141 (RR141) in water was investigated over iron containing ZSM-5 zeolite (Si/Al = 42) prepared by ion-exchange (FeZSM-5 (42)). The catalyst was characterized by XRD, SEM, FTIR, TPR, and ICP-AES measurements. The effects of the initial concentrations of the dye and H2O2, the initial pH of the solution, catalyst loading, and the reaction temperature were investigated on heterogeneous Fenton-like degradation of RR141. The reduction of the solution initial pH from ca. 7.0 to ca. 3.5 had a positive effect on color removal. A complete color removal was achieved with all the H2O2 concentrations in the range of 0.007 - 0.067 M over the FeZSM-5 (42) catalyst after 2 h of reaction. The COD reduction increased from 52% to 81% with an increase in the amount of the catalyst. The COD reduction was affected positively with the increase in temperature from 298 K through 313 K to 323 K and then to 333 K. The initial decolorization rate was described by the equation: −rA0 = 9.4*104 e-38.8/RT CRR141,0 CH2O2,0 0.184 with an H2O2 concentration range of 0.007 M – 0.033 M (where R is in kJ/mol).
Sulfonated and unsulfonated azo dyes have a negative aesthetic effect on the wastewater that is highly colored even at a low concentration of dye. On the other hand these dyes are toxic, carcinogenic and mutagenic. It is difficult to remove azo dyes in wastewater produced by textile industries using biological, physical and chemical treatment methods because of the chemical stability of these dyes, the high cost of the processes, and also disposal problems. Therefore, it is necessary to find an effective method for the wastewater treatment of reactive azo dyes. In the last decade, attention has focused on the Advanced Oxidation Processes (AOP) that is based on the generation of highly reactive hydroxyl radicals.
Decolorization of the dye is a result of N = N bond destruction with the addition of OH.. The mineralization of dye is the total oxidation of the intermediate products to CO2 and H2O and it is slower than color removal because of the priority of the OH. attack on the N = N bonds .
The degradation of RR141 has been investigated by biodegradation [27-29], by adsorption [22,30,31], by homogeneous Fenton’s reaction, by non-catalytic or catalytic photooxidation [32-41], by electrochemical oxidation with conductive-diamond anode , and by ultrasound . Few studies have been reported on the heterogeneous Fenton-like degradation of C.I. Reactive Red 141 to date. In one study, iron oxide particles recovered from acid mine drainage were used as an adsorbent or as a catalyst in the oxidation of RR141 through a Fenton-like mechanism to remove the dye from the aqueous solution . However, the main aim of that study was to investigate the dye-adsorption capacity of iron oxide rather than its catalytic effect in the heterogeneous Fenton-like oxidation of dye. Only one experiment has been carried out for dye degradation by heterogeneous Fenton’s reaction and a TOC removal of around 3% could only be achieved.
Conventional processes such as adsorption, coagulation/flocculation (CF) etc., may be costly, ineffective and produce a high amount of secondary wastes. CF is still not good enough to be used in industry even when it is combined with microfiltration or ultrafiltration. However, catalytic methods such as heterogeneous Fenton-like oxidation result in permanent chemical degradation of dyes. This process is still simple, non-expensive, a promising, and attractive treatment method for the effective decolorization and degradation of dyes when compared with the conventional processes [25-43].
Many studies are found in literature on the removal of dyes using Fe-ZSM-5 [3,23,24,44], Fe-Y [2,25,45-48], and Fe-clay [26,49-52] catalysts by several advanced oxidation techniques. The catalytic activity and stability of these catalysts depend on the synthesis method in addition to their composition and framework structure. The leakage of iron ions from the support is the other important factor to be considered in dye degradation over an iron containing support: because iron leaching from the catalyst causes a new pollution of the treated water. The studies showed that iron containing ZSM-5 zeolite exhibited better catalytic activity and stability than iron-containing Y zeolites. On the other hand, the activity of iron-containing clay catalysts in the degradation of dyes depends on the careful selection of the preparation method and calcination conditions. However, till now no a detailed parametric study including decolorization kinetics has not been reported on the heterogeneous Fenton-like degradation of dyes on iron containing ZSM-5 zeolites. The objectives of this study are to: (1) investigate the influence of the reaction conditions of the heterogeneous Fenton-like oxidation and optimize them, (2) investigate the decolorization kinetics, and (3) investigate the leakage of iron ions in the reaction for the stability of the catalyst.
Our group previously published a study  on the degradation of RR141 using the heterogeneous Fenton-like process over iron containing ZSM-5 zeolites. That work included the preparation of the catalysts by ion-exchange or hydrothermal synthesis and their characterization studies by XRD, SEM, FTIR, ICP-AES, TPR, and nitrogen adsorption. The catalytic activity screening tests of the prepared catalysts were accomplished to determine the catalyst with the highest activity in the degradation of RR141 by heterogeneous Fenton-like oxidation reaction. The highest color removal (97%) was achieved by the catalyst prepared by ion exchange with a silicon/aluminum ratio of 42 zeolite (FeZSM-5(42)). The above mentioned objectives of the presented study was investigated over that iron-containing ZSM-5 zeolite catalyst. The presented study is novel and unique from these points of view.
Preparation of the catalysts
Ion exchange was used for the preparation of the iron containing the ZSM-5 zeolite catalyst. The method of Schwidder et al.  was applied with minor modifications  for the ion-exchange. The ZSM-5 zeolite with silicon/alumina = 42 was obtained from Süd-Chemie AG (Germany). An iron exchange of 98.9% could be achieved. The catalyst was coded as FeZSM-5 (42).
The prepared catalyst was characterized by nitrogen adsorption, X-ray diffraction patterns (XRD), scanning electron microscope (SEM), Fourier transform-infrared (FTIR) spectrometer, inductively coupled plasma atomic emission spectrometer (ICP-AES), and by temperature programmed reduction (TPR) measurements. The precise procedures for the characterization of the catalyst are described in Ref .
Heterogeneous Fenton-like oxidation of RR141
The decrease of the intensity of the band at 543 nm was used as a measure of decolorization degree. The reduction in the chemical oxygen demand (COD) of the dye solution was determined using a Lovibond (Germany) Checkit Direct COD Vario device for each run after a reaction time of 2 h.
The blank run with the above conditions, but without H2O2 showed that dye removal by adsorption was not greater than 3% and 21% in 15 min and 120 min of reaction, respectively. A color removal of 11% could be achieved in the presence of H2O2 only in 2 hour of reaction.
Each experiment was conducted in duplicate and the standard deviation of the average of the independent runs for color removal changed in the range of ±0.51 to ±1.29.
Results and discussion
Catalyst characterization studies
The X-ray diffraction patterns of the FeZSM-5 catalyst sample showed the typical diffractrograms of the MFI structure (2θ = 7-90 and 23-250). The incorporation of iron in the MFI lattice did not damage the zeolite structure .
Iron content and Si/Al ratio of the catalyst were determined with the ICP-AES method and found to be 4.98 wt% and 42.8, respectively. The BET surface area, total pore volume, average pore diameter and micropore area of the catalyst were found to be 469 m2/g, 0.321 cm3/g, 0.73 nm (using the Horvath-Kawazoe method), and 236 m2/g, respectively.
The FTIR spectra of the catalyst showed bands at 450, 550, 800, 1100, 1225, and 1650 cm−1 which were assigned to different vibrations of the tetrahedral and framework structure of the ZSM-5 zeolite .
The temperature-programmed reduction with hydrogen (H2-TPR) of the catalyst showed that a major hydrogen consumption peak was obtained at 397 K which reflected the reduction of out of framework iron oxides .
Influence of the initial pH of solution on the degradation of dye
The effect of solution pH on the degradation of dye was investigated at an initial dye pH of ca. 7 and at a pH of 3.5 which was regulated by the addition of 0.1 N sulphuric acid to the dye solution.
The amount of iron loss from the catalyst into the solution was determined by measuring the iron concentration in the solution after a reaction duration of 2 h, with an atomic absorption spectrophotometer (Varian 10 plus). The leaching of iron cations from the zeolite into the solution depended strongly on the pH . As expected, with the regulation of pH from 7 to about 3.5 the iron leaching increased from 0.3×10−3 g/dm3 to 0.9×10−3 g/dm3. It means that iron loss changed from 0.59% to 1.77%. As seen, the iron leaching was considerably low (being below the EU directives of < 2×10−3 g/dm3).
Influence of the hydrogen peroxide concentration on the degradation of dye
The dominant response from the two opposite effects given in Equations 1 and 7 directs the reaction. Similar results have been reported by Neamtu et al.  and Ramirez et al. , in the Fenton-like oxidation of Procion Marine H-EXL and Orange II, respectively.
Figure 5b presents the percentages of decolorization and COD removal in the degradation of RR141 after a reaction time of 2 h. COD reduction reached 57% in the presence of 0.067 M of H2O2, while it was 54% at a dose of 0.007 M H2O2 and decreased to 38% with the increase in H2O2 concentration from 0.007 M to 0.033 M. A COD removal of 52% was obtained at a dose of 0.267 M H2O2. The COD removal is significantly lower than the color removal at all doses of H2O2. This result signifies the priority of the OH. attack on the N = N bonds and the slower destruction of the aromatic/olefinic carbons in the dye . For cost considerations, the optimum H2O2 concentration can be selected as 0.007 M.
In literature, the COD (chemical oxygen demand), TOC (Total Organic Carbon), and DOC (dissolved organic carbon) removals were measured in the degradation of RR141 by several advanced oxidation techniques. For instance a TOC removal of about 3% was achieved in the heterogeneous Fenton-like oxidation of RR141 over iron oxides particles recovered from acid mine drainage .
A 17%-23% TOC removal was achieved in the degradation of RR141 by the ferrioxalate-Fenton/UV-A and TiO2/UV-A processes .
A 100% DOC removal was obtained for RR141 after a 90 min treatment under homogeneous Fenton assisted solar light .
A decrease of 64% in COD was reached in the degradation of RR141 within 5 hours using the UV/H2O2 advanced oxidation process .
COD was reduced from 120 mg/L to 23 mg/L (81%) in the solar nano-photocatalytic degradation of RR141 using TiO2 .
A 37% removal of TOC was achieved in the photocatalytic degradation of RR141 for the Zn2SnO4 photocatalyst after 270 min of sunlight irradiation .
A TOC reduction of 29% was achieved in the degradation of RR141 with a TiO2 coated pebble bed photocatalytic reactor having a solar collector .
A COD removal of 100% was obtained in the electrolyse of an aqueous solution of RR141 with a conductive-diamond anode .
The influence of the catalyst amount on the degradation of dye
Influence of the temperature on the degradation of dye
In literature, similar results have been reported in the catalytic wet peroxide oxidation (CWPO) of Orange II over an Fe-saponite catalysts , in the CWPO of phenol over pillared clays containing iron  and in the wet oxidation of 2.4.6-trichlorophenol in water using an Fe3+, Co2+, Ni2+ supported MCM-41 catalysts .
Stability of the catalyst
Decolorization kinetics of the Fenton-like oxidation of RR141
In the Fenton-like oxidation of RR141, the reaction mixture was stirred vigorously at around 280 rpm. The external diffusion effects were calculated using Hougen’s criterion and it was found that (Cb-Cs)/Cb ≈ 0.04, so it was assumed that Cb ≈ Cs. The internal diffusion resistance was negligible due to the small size of the catalyst particles (500 nm). To calculate the internal diffusion effects, the generalized Thiele modulus based on the reaction rate was determined and found to be 0.339×10−6 and hence the effectiveness factor was assumed to be unity .
The decolorization kinetics was determined at an initial pH of 3.5 using the initial decolorization rates and a first order dependency was obtained on the dye concentration with R2 = 1. This result was in good agreement with those reported in literature for decolorization kinetics of RR141 degraded by several advanced oxidation techniques [1,32,34,37,38,40,59]. However, the photo-catalytic degradation of RR141 on Zn2SnO4 followed the zero order kinetics under sunlight .
Reaction rate constants at different temperatures
Temperature (T), K
-r A0 (mol/dm 3 .min)
k (dm 3 /mol) 0,184 min −1
C RR141 (mol/dm 3 )
C H2O2 0,184 (mol/dm 3 ) 0.184
In literature, the activation energy for the heterogeneous Fenton-like reaction of RR141 has not been declared. This study is a useful reference in the decolorization kinetics of RR141 for the design of RR141 removal reactors. In the homogeneous photo-Fenton reaction of RR141, activation energy was estimated to be 1.26 kJ/mol . The lack of mass transfer resistances facilitates the homogeneous catalytic reactions with low activation energies. Decomposition of RR141 with the ferrioxalate-Fenton/UV-A process was fitted to the empirical Langmuir-Hinshelwood kinetic model . An activation energy of 35.9 kJ/mol was reported for the rapid decolorization of azo dye methyl orange in an aqueous solution by nanoscale zerovalent iron particles . This value is very close to the activation energy (38.8 kJ/mol) obtained in this study for the heterogeneous Fenton-like oxidation of Reactive Red 141. Moreover, in literature, the activation energy of the homogeneous catalytic Fenton oxidation of Reactive Brillant Blue X-BR azo dye was given to be 25.21 kJ/mol .
The heterogeneous Fenton-like degradation of Reactive Red 141 (RR141) in water was investigated over iron containing ZSM-5 zeolite (Si/Al = 42) prepared by ion-exchange. The catalyst seems to have a promising efficiency in RR141 degradation. A complete color removal could be achieved with the catalyst at a pH of 3.5 in an H2O2 concentration range of 0.007 M-0.067 M after two hours of reaction. The increase in H2O2 concentration up to 0.033 M increased the initial decolorization due to the increase of the OH. radicals formed. However, at H2O2 concentrations higher than 0.033 M the initial decolorization rate of RR141 was decelerated. The highest COD removal was obtained to be 81% with a complete color removal at an H2O2 concentration of 0.267 M and at 333 K with a catalyst amount of 0.3 g for 0.15 dm3 a dye solution of 0.1 g/dm3. An increase in temperature positively affected the decolorization of dye as well as the COD removal. The initial decolorization rate was described as -rA0 = 9.4*104 e-38.8/RT CRR141,0 CH2O2,0 0.184 in the H2O2 concentration range of 0.007 M – 0.033 M. Iron leaching remained below the EU directives. The small iron leaching makes it possible for the catalyst to have long term stability without generating iron hydroxide sludge.
It can be concluded that this study offers a significant potential for the application of heterogeneous Fenton-like oxidation over iron containing a ZSM-5 zeolite for the degradation of RR141 aqueous solutions. It will be a good alternative to the oxidation methods currently used in the degradation of RR141.
The authors acknowledge the financial support from TÜBİTAK (The Scientific and Technological Research Council of Turkey) under Project number of 108 M175 and from the Ege University Scientific Research Fund under project number of 08MÜH023.
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