ࡱ> q`)bjbjqPqP q,::\CDGK""".I0I0I0I0I0I0I$ILhNDTI%}!0"%%TIoK,,,%.I,%.I,, EF V3]*EH4K0GKEN{+xN0FNFT"?#h,#T#"""TITI, """GK%%%% LABORATORY STUDY OF THE FENTON AND PHOTO-FENTON OXIDATION TREATMENT OF LAS SURFACTANT WASTEWATER S. PAPI, N. KOPRIVANAC, I. PETERNEL, D. VUJEVI, I. GR I University of Zagreb, Faculty of Chemical Engineering and Technology, Maruliev trg 19, HR-10000 Zagreb, Croatia ABSTRACT The present study investigates the treatment of surfactant wastewater by the advanced oxidation processes of Fenton type. Synthetic solutions of linear alkylbenzene sulfonate (LAS), as a model compound commonly used in the formulation of detergents and present in industrial wastewaters, are investigated in this work. Experiments were conducted at LAS concentration of 100 mg dm-3. The mineralization of LAS synthetic wastewater has been studied using Fe2+/H2O2, Fe3+/H2O2, Fe2+/H2O2/UV and Fe3+/H2O2/UV processes. The extent of mineralization was determined on the basis of total organic carbon (TOC) measurements. Batch experiments for Fenton and photo-Fenton oxidation were performed in water jacked cylindrical reactor of 0.5 dm3 capacity. For photo-Fenton oxidation a low pressure mercury lamp (125 W) which emits at 254 nm was used. Experiments were carried out to investigate the optimal operational conditions of the process: H2O2 dosage, Fe2+ and Fe3+ concentration, optimal Fe2+/H2O2 and Fe3+/H2O2 ratios. Mineralization rates in all processes were determined. The mineralization of LAS expressed as a percentage of TOC remaining after the treatment (TOC/TOC0, %) was found to be: 53 % for Fe2+/H2O2, 51 % for Fe2+/H2O2/UV, 67 % for Fe3+/H2O2, and 48 % for Fe3+/H2O2/UV process with 0.005 M Fe2+ or Fe3+ dosage and 1 : 20, Fe2+ or Fe3+/ H2O2 molar ratio. Keywords: wastewater treatment, AOPs, Fenton type processes, UV irradiation 1. INTRODUCTION The water and wastewater pollution control is one of todays main fields of scientific activity. More and more the ecosystem is loaded with large quantities of surfactants, which are the main component of widely used household detergents. Surfactants have also been widely used in textile, fiber, food, paints, polymers, plant protection, cosmetics, pharmaceuticals as well as mining, pulp and paper industries [1]. Among wide range of surfactant types, linear alkylbenzene sulfonate (LAS), the most common synthetic anionic surfactant used in domestic and industrial detergents, has a global production of about 2.4 106 tonnes per year [2]. LAS is produced by sulfonation of linear alkylbenzene with sulfur trioxide. LAS is a mixture of closely related isomers and homologues, each containing an aromatic ring sulfonated at the para position and attached to a linear alkyl chain with the length which varies between C10 and C14 [3]. Detergents usually contain 5 - 25 % of LAS. From the environmental point of view, it is the major anthropogenic source of organic compounds in primary sludge of the municipal wastewater treatment plants. It can be adsorbed onto suspended solids ranging from 30 to 70 % and, hence, escaping aerobic treatment [4]. It has also been identified in surface water supplies in the concentrations lower than 1 g dm-3 [5], and in the drinking water with the concentrations of 0.001 - 0.008 mg dm-3 [3]. It has been reported that LAS at higher concentrations, between 20 and 50 mg dm-3, such as in detergent manufacturing wastewaters, is not biodegradable [6, 7, 8]. It is implied that some of chemical processes need to be used to degrade aqueous LAS. Among these processes advanced oxidation processes (AOPs) are attractive alternatives for the treatment of wastewater containing bioresistant compounds. AOPs are processes that produce highly reactive intermediates, mainly hydroxyl radicals (OH), which are able to oxidize almost all organic pollutants to CO2 and H2O [9]. An alternative advanced oxidation method which achieves high efficiency with a low treatment cost would be highly desirable. The methods meeting these requirements are Fenton and photo-Fenton processes. These AOPs have been successfully applied for the treatment of the surfactant wastewater [1]. Fenton and photo-Fenton reactions are AOPs where oxidant species are generated from hydrogen peroxide and Fe2+/Fe3+ as a catalyst [10]. In Fenton reaction ferrous salts react with hydrogen peroxide and generate the hydroxyl radicals as follows (reaction 1): Fe2+ + H2O2 ! Fe3+ + HO + HO- (1) Then, Fe3+ can be reduced by reaction with exceeding H2O2 to form ferrous ion again and additional amount of hydroxyl radicals. This second process is called  Fenton like process . It is slower than Fenton reaction and allows Fe2+ regeneration giving the place to a catalytic mechanism (reactions 2 -4): Fe3+ + H2O2 ! FeOOH2+ + H+ (2) FeOOH2+ ! HO2 + Fe2+ (3) Fe3+ + HO2 ! Fe2+ + O2 + H+ (4) The rate of contaminant s degradation can be considerably increased via photochemical reaction in the photo-Fenton process. In this case, the regeneration of Fe2+, with additional production of HO radicals, is followed by photoreduction process (reactions 5 and 6): Fe3+ + H2O ! FeOH2+ + H+ (5) FeOH2+ + h ! Fe2+ + HO  < 410 nm (6) The UV irradiation radiation (UV-C 254 nm), was used to enhance degradation (mineralization) of LAS surfactant present in synthetic wastewater. The aim of this study was to investigate the optimal process parameters (H2O2 dosage, Fe2+ and Fe3+ concentrations, optimal Fe2+/H2O2 and Fe3+/H2O2 molar ratios), and to determine mineralization rates as well as the overall process efficiency. 2. EXPERIMENTAL Materials Model solution of sodium salt of dodecylbenzene sulfonic acid (Aldrich) was used to study the degradation characteristics of LAS. This alkyl chain contains 12 carbons with molecular weight of 348.48. The initial concentration of LAS for all the experiments was 100 mg dm-3 (TOC0 = 48.49 mg dm-3). FeSO4 7H2O (Kemika), Fe2(SO4)3 9H2O (Kemika), H2O2, 30 % w/w (Kemika), Na2S2O3 (Gram-mol), starch (C6H10O5)n (Kemika), KI (Kemika) and (NH4)6Mo7O24 4H2O (Kemika) were used as reagent grade. The pH of the reaction system was adjusted using 25% H2SO4 and 50% NaOH solutions. Photoreactor Batch experiments, for Fenton and photo-Fenton oxidation were performed in a cylindrical photoreactor of 0.5 dm3 capacity. The reactor was made of borosilicate glass, with sampling ports on the top, magnetic stirrer and water jacked for temperature control. For photo-Fenton oxidation a low pressure mercury lamp (125 W, UV-C 254 nm) was placed axial in quartz tube inside of the reactor. Analysis Experiments of Fenton oxidation were carried out as follows: required amount of Fe2+ (or Fe3+) was added into the 500 cm3 of LAS solution; pH was adjusted to pH = 3 using pH-meter Schott Instruments GmbH; than required amount of H2O2 was added; UV lamp was turned on for photo-Fenton process, the solution was mixed for 60 minutes. Samples of LAS solution were taken during the process, at periodic intervals, and measurements were carried out with TOC-VCPN, Total Organic Carbon Analyzer, SHIMATZU. The residual hydrogen peroxide was determined by the standard method [11]. 3. RESULTS AND DISCUSSION A first set of experiments was performed in order to establish optimal molar ratio (Fez /H O ) for the highest LAS mineralization extents (Figure 1). The lowest residual TOC extent; 46% was achieved at molar ratio (Fez /H O ) 1:100. Also, it can be seen that similar LAS mineralization extents can be accomplished using different molar (Fez /H O ) ratios. Thus, variation of the molar ratio (1:1, 1:20, 1:50 and 1:100) for fixed ferrous salt concentration (0.005 M) caused only minimal change on the final mineralization extents in terms of residual TOC (46 - 54%). Molar ratio Fez /H O of 1:20 has been declared as optimal on the basis of the highest TOC removal, because further increasing of the H2O2 concentration (1:50, 1:100) did not show any benefit in the final process efficiency but at the same time increased unnecessary the larger amount of H2O2 consumption.  Figure 1. Influence of Fe2+/H2O2 ratio on LAS surfactant mineralization in Fenton oxidation with 0.005 M Fe2+ dosage The influence of FeSO4 7H2O concentration alone and in the combination with hydrogen peroxide on LAS mineralization efficiency was shown in Figure 2. Rather small influence of Figure 2. Influence of Fe2+ dosage on LAS surfactant mineralization without addition of H2O2 and with 0.1 M H2O2 dosage higher FeSO4 7H2O concentration on final LAS mineralization extent was noticed. That fact is maybe consequence of parallel coagulation effect occurred in solution. Namely, for the concentration of Fe2+ salt 0.005 M, residual TOC extents is about 80%, but Fenton process (Fez /H O ) is showing higher process efficiency using the same Fe2+ salt concentration with residual TOC extent about 50%. Further increase of Fe2+ salt concentration causes only small decreasing of residual TOC value until it reaches maximal, constant extent.  Figure 3. Influence of H2O2 dosage on LAS surfactant mineralization without addition of Fe2+and with 0.005 M FeSO47H2O dosage With the Figure 3 the influence of initial H2O2 concentration on LAS mineralization efficiency in terms of TOC removal has been described. Namely, 0.1 M concentration of H O was found to be optimal one with residual TOC extent of 70%, while further increase of H2O2 concentration did not affect final process efficiency increase. Also, Fez /H O process showed maximal mineralization extents at 0.1 M H2O2, so this initial peroxide concentration was found as optimal for the highest mineralization efficiency with residual TOC extent about 45%. Further increase of H2O2 concentration did not benefit in the mineralization efficiency. This can be explained with the fact that Fez ions did not react with H2O2 molecules in order to produce hydroxyl radicals only, but they also consumed HO radicals during the process (scavenger effect) causing decrease of the total process efficiency [12].  Figure 4. Kinetics of LAS surfactant mineralization in Fe2+/H2O2 process with 0.005 M Fe2+ dosage and Fe2+/H2O2 ratio adjusted at 1:20; with and without UV light The next set of experiments was performed in order to describe LAS mineralization kinetics by Fez /H O process. Figure 4 shows results of LAS mineralization kinetics by Fenton process with and without UV irradiation as well as the effect of gradually added ferrous (II) salt on the final LAS removal from the water. The same amount of ferrous (II) salt was added again into the reaction system after 20 minutes of regular Fenton treatment. As it can be seen from Figure 4, this re-addition caused a small increase in the final process efficiency. Reaction kinetics and LAS mineralization rate could also be compared for both processes, Fenton and UV/Fenton. It could be estimated clearly that presence of UV irradiation positively affected the efficiency of the Fenton treatment. In the first 10 minutes of the treatment by Fenton process, reaction kinetics as well as mineralization extents are similar for the cases with and without UV irradiation. After 10 minutes of treatment the difference between those two processes (Fenton and UV/Fenton) has become rather obvious. After 60 minutes of UV/Fenton treatment residual TOC extent was lower (50 %) in comparison with Fenton process in dark (65 %). Fenton like process, Fe3+/H O , was applied for the mineralization of LAS too. Mineralization rate is higher for Fe2+/H2O in comparison with Fe3+/H O because Fe3+ must be reduced into Fe2+ before it starts to produce hydroxyl radicals during the Fenton process. Experimental work of this study has showed no specific influence of ferrous and ferric salts (Fe2+ or Fe3+) on LAS mineralization rate. The Fez / H O molar ratio was found as dominant parameter influencing LAS mineralization rate (Figure 5.). From the Figure 5 it can be seen that highest surfactant mineralization extent was achieved at molar ratio 1:1 with residual TOC 47 %. Increase of molar ratio (1:20, 1:50, 1:100) caused decrease of the mineralization extent. Possible explanation can be the scavenger effect discussed earlier in this paper. Figure 5. 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It is obvious that ferrous (III) sulphate has significant influence on LAS removal from the water. Mineralization extents in terms of residual TOC are in the range of 27 to 34 % at different Fe3+ concentrations. Residual TOC extents are much higher in the case of Fez /H O process; 58-73 %. Also, it can be noticed that increase of Fez concentration over 0.005 M caused no improvement in final process efficiency. It is interesting to point out that coagulation effect with Fe3+ is much more efficient than Fenton oxidation with Fenton like process, Fez /H O .  Figure 6. Influence of Fe3+ dosage on LAS surfactant mineralization without addition of H2O2 and with 0.1 M H2O2 dosage H O independently is causing partial mineralization of LAS surfactant even in a very small concentration, 0.002 M, with residual TOC about 80%. Further increase of hydrogen peroxide concentration does not affect on LAS mineralization efficiency. Figure 7 shows the influence of hydrogen peroxide concentration in Fenton like process with constant Fe3+ concentration. Again, the maximal process efficiency in terms of residual TOC extent was achieved at lower H2O2 concentration, 0.002 M with residual TOC = 45 %. The further investigation was directed to determine LAS mineralization kinetic using Fez /H O process with and without presence of UV irradiation and the results are presented in Figure 8. Maximal LAS mineralization rate was achieved in first 10 minutes. As it was  Figure 7. Influence of H2O2 dosage on LAS surfactant mineralization without addition of Fe3+and with 0.005 M Fe2(SO4)39H2O dosage  Figure 8. Kinetics of LAS surfactant mineralization in Fe3+/H2O2 process with 0.005 M Fe3+ dosage and Fe3+/H2O2 ratio adjusted at 1:20; with and without UV light expected UV assisted Fenton process was much more efficient in terms of residual TOC; 70 % for the dark Fenton process despite 50 % of TOC removal for the UV/Fenton process. Figure 9 shows results of the remaining H2O2 after the Fenton oxidation. Excess of H2O2 was shown as a percentage of the amounts on the beginning of the processes. As it can be seen from Figure 9 percentage of the remaining hydrogen peroxide after the Fenton oxidation is different for all molar ratios except ratio 1:1. At this molar ratio 40 % of remaining H2O2 was found for both processes. Maximal consumption of hydrogen peroxide (90 %) was noticed in the case of Fez /H O process at molar ratio 1:20. It can be concluded that maximal consumption of hydrogen peroxide was used for generating OH radicals which are necessary for LAS degradation. For all other investigated molar ratios the percentage of remaining hydrogen peroxide is higher. Figure 9. Percentage of residual H2O2 after treatment by Fe2+/H2O2 and Fe3+/H2O2 processes at different Fe2+ or Fe3+/H2O2 ratios (initial concentration of ferrous and ferric ion was 0.005 M) 4. CONCLUSIONS The aqueous LAS was degraded in a batch photoreactor by Fenton and photo-Fenton type of advanced oxidation processes using ferrous and ferric salts. About 50 % of initial LAS organic content was degraded towards mineralizationLdfjlnp*,68Z^xzBTˆ(.0468:<>@BN˹ˮ◌yh[mH sH hIh[mH sH jhIhIUhOhmH sH h2MhI .OJQJmH sH h2MhI .mH sH hI .H*mH sH hhH*mH sH hI .mH sH h2MhOhOJQJmH sH h2MhOhmH sH hWlmH sH hhmH sH U/DFHJLNP@B#fjlnprtvx?AB $da$gdom|d^`|gdA $da$gdK{z|d^`|gdK{z $da$gd)NPbd*,.0>@BDFHJ"&'+bgo| #(:W ʿh2MhOhH*mH sH h2MhOhH*mH sH hmH sH hAmH sH h2MhOhOJQJmH sH h2MhOhmH sH  hK{zhK{zhIhi)hK{zH*hi)hK{zH* hK{zH* huhK{zhK{zh2Mh[mH sH 5Pdfhjtx#+,/01256?@ADEFIǼwl`lhomhomH*mH sH homhommH sH hommH sH  hAhomhom homh):jhomhomUhAmH sH hAhAH*mH sH hAhAH*mH sH hAhAmH sH h):mH sH h):hK{zmH sH jh):h):UhK{zmH sH h2MhOhmH sH hAmH sH  BCDEFGHIߖ|d^`|gdjdgdo?j $da$gdW $da$gdg|d^`|gdom $da$gd)EFLPnoőƑǑɑ-<>RS º²º²§››››““²²››²„„„h2MhOhOJQJmH sH hWlmH sH h2MhOhH*mH sH jhghgUhAmH sH hmH sH h2MhOhmH sH  homhomhomhomH*mH sH hommH sH homhommH sH homhomH*mH sH 4 ̔Д>?@CXZ\]^`giklmpؖޖߖǼڴ~rh2MhEL5mH sH h2MhjmH sH hjmH sH hjhjH*mH sH hjhjH*mH sH hjhjmH sH ho?jmH sH h2MhgmH sH hgmH sH hghgmH sH hOhmH sH h2Mh$FmH sH hmH sH h2MhOhmH sH +aˮ-wx)$hd^h`a$gdo?j$hd^h`a$gdD $da$gd{$hd^h`a$gd{ $da$gdW $da$gdELҗMQcdy{}~¬ì֬ެ 67ݸݬݠݬݬݠݬݬݠݬݬݠݬݬݠݠݠݠݬݬ—Œh&hNmH sH h&H*mH sH h2MhNH*mH sH h2MhNH*mH sH hAmH sH Uh&mH sH h2MhAmH sH hmH sH h2MhNmH sH h2MhmH sH h2Mh5mH sH 7. The mineralization of LAS expressed as a percentage of TOC remaining after the treatment (TOC/TOC0, %) was: 53 % for Fe2+/H2O2, 51 % for Fe2+/H2O2/UV, 67 % for Fe3+/H2O2, and 48 % for Fe3+/H2O2/UV process with 0.005 M Fe2+ or Fe3+ dosage and 1 : 20, Fe2+ or Fe3+/ H2O2 molar ratio. The result of 67 % TOC/TOC0 for model LAS solution could be a solid base for further investigations of AOPs application for such systems. 5. REFERENCES [1] Lin, S.H., Lin, C.M., Leu, H.G.; Wat. Res. 33(7), (1999) 1735. [2] Dealmedia, J.L.G., Dufaux, M., Taarit, Y.B., Naccache; C.; J. Am. Oil Chem. Soc. 71(7), (1994) 675. [3]  HYPERLINK "http://www.heraproject.com/RiskAssessment" http://www.heraproject.com/RiskAssessment. [4] Berna, J., Ferrer, J., Moreno, A., Prats, D., Bevia, F.; Tenside Surfac Det., 26, (1989) 101. [5] Tabor, C.F., Barber, L.B.; Environ. Sci. Technol., 30(1), (1996) 161. [6] Tabrizi, G.B., Mehrvar, M.; Sep. Purif. Technol., 49, (2006) 115. [7] Zhang, C.L., Valsaraj, K.T., Constant, W.D., Roy, D.; Wat. Res., 33(1), (1999) 115. [8] Patterson, D.A., Metcalfe, I.S., Xionf, F. Livingston, A.G.; Ind. Chem. Res., 40, (2001) 5507. [9] Kang, S.F., Liao, C.H., Chen, M.C.; Chemosphere, 46, (2002) 923. [10] Nunez, L., Garcia-Hortal, J.A., Torrades, F.; Dyes Pigments, (2006) in press [11] Clesceri, L.S., Eaton, A.D., Greenberg, A.E. (eds.); Standard methods for the examination of water and wastewater, APHA, AWWA & WEF, Waldorf, MA, pp. 3-76, 5-16, 1998. 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