Oxidative decolourization of Rhodamine-B using sea nodule residue

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1 Indian Journal of Chemical Technology Vol. 21, July 2014, pp Oxidative decolourization of Rhodamine-B using sea nodule residue P K Satapathy 1, *, Marina Das 1 & A K Sahoo 2 1 P G Department of Chemistry, North Orissa University, Baripada , Odisha, India 2 Department of Chemistry, F.M. Junior College, Balasore , Odisha, India Received 29 November 2012; accepted 28 February 2014 The characterization of sea nodule leached residue catalyst has been done by various physicochemical methods, such as XRD, FT-IR and surface area measurement. The oxidative decolourization of Rhodamine-B (Rh-B) by sea nodule residues is studied in batch technique. The extent of decolourization increases with increase in catalyst dose while decreases with the increase in initial ph of the solution and dye concentration. More than 93% of 5 mg/l Rh-B is decolourized within 1 h with a catalyst dose 0.5 gm/l at ph ~ 3. Keywords: Decolourization, Rhodamine-B, Sea nodule residue The adsorptive properties and catalytic activities of manganese nodules for adsorptive removal of various pollutants and degradation of organic substrates are well studied The selective extraction of strategic metals like Cu, Co and Ni from these manganese nodules produces more than 70% residue as wastes for disposal. These leached residues containing oxides/oxyhydroxides of Fe, Mn, Al and Si show reasonable high porosity and surface area. Moreover, Fe and Mn in these residues are present in variable oxidation states. In view of above characteristics, one can study the use of leached residues as an effective oxidation catalyst for a variety of organic pollutants. Recently the adsorption properties and catalytic activity of sea nodule residues have been carried out for the removal of various pollutants and degradation of organic dyes The removal of toxic pollutants from wastewater is an important and widely studied research area. Rhodamine-B (Rh-B) is considered to be a hazardous pollutant due to its toxic nature even at low concentration, and non-biodegradability character. Rh-B is the persistent pollutants that have been used as coloring agents in chemical, textile, pulp and paper, printing cosmetics, leather and food industries 23,24. The various effective techniques applied for Rh-B removal from wastewater are reverse osmosis, biological degradation, chemical oxidation, precipitation, electro dialysis and adsorption 25,26. Usually, the treatment * Corresponding author. pramoda_satapathy_70@yahoo.com methods for dye effluents include homogeneous oxidation such as UV/O 3 and H 2 O 2 /Fe and heterogeneous photocatalytic oxidation using cds 28. Since these methods are not cost effective, photo-oxidative decolourization of red F3B dye is employed by Liu and Tang 29. In the present investigation, the oxidative decolourization of Rhodamine-B using sea nodule residue has been studied. Experimental Procedure Sea nodule residues (SNR), generated after reduction roast-ammoniacal leaching process was collected from Pilot plant operated at Hindustan Zinc Limited, Udaipur, India. The parent Indian Ocean manganese nodule (SN), which generates the residue after leaching process, was also collected for comparison of activity. The samples were air dried for several days, mixed thoroughly and kept in airtight bottles for characterization and further use. In order to remove loosely associated metal ions/anions, the leached residue was washed with distilled water. In a typical lot 50 g of the leached residue was dispersed in 500 ml distilled water (solid : liquid ratio = 1 : 10) and stirred for 2 h at room temperature. The content was filtered, washed with distilled water for further removal of sulphate and then air dried to get the washed sea nodule residue (WSNR). These samples were used for oxidative decolourization of Rhodamine-B. Characterization of samples Chemical analyses for major and minor constituents in different samples were done as

2 258 INDIAN J. CHEM. TECHNOL., JULY 2014 described earlier by conventional wet chemical methods and by atomic absorption spectrometer (Avanta, GBC), respectively 30. Particle size of SNR and WSNR was determined using Malvern SA-CP3 particle size analyzer. The XRD patterns of samples were recorded on a Sidemen s D 500 X-ray diffractometer using CuK α (λ = ) radiations. FTIR spectra of different samples in KBr pellets were recorded using a ThermoNicolet 870 FT-IR in absorption mode averaging 32 scans and at a resolution of 4cm -1. Surface areas of the samples were determined by N 2 /BET method using a Quantasorb (Quantachrome, Novawin). All ph measurements were carried out by a Toshniwal CL 54 ph meter using a combined glass electrode. Chemicals Stock solutions of Rhoda mine-b were prepared in distilled water. Working solutions were prepared by suitable dilution of stock with distilled water. Oxidative decolourization of Rhodamine-B Decolourization of Rh-B was conducted in batches at constant temperature (25 ± 1.0 C) using a water bath. An accurately weighed quantity of residue was added to a 500 ml stirred dye solution taken in a 3-necked round bottomed flask equipped with a magnetic stirrer. The dye concentration was kept in the range mg/l while the initial ph values were adjusted in the range At specific time intervals, aliquots of 10 ml suspension were withdrawn and centrifuged to separate the catalyst particles and the concentration of residual dye was measured at 554 nm using UV/Visible spectrophotometer. Residual content of the dye was calculated using the following formula: Residual content (n), % = (C t /C o ) 100 where C t is the dye concentration at time t; and C o, the initial concentration of the dye under study. The influence of ph of suspension, dye concentration and loading of the residue, on decolourization of Rh-B was studied. Results and Discussion Characterization of leached residue Particle size analyses show that the leached residue contains very fine particles with mean particle diameter of 17.8 µm. The BET surface areas of SN, SNR and WSNR are found to be 130, 60.9 and 66.7 m 2 g -1 respectively. Decrease in surface area of SNR is presumably due to the loss in porosity of SN and formation of manganese carbonate and silicate on roasting of SN with coal. Marginally higher surface area of WSNR is presumably due to the increased number of accessible pores on washing of adsorbed species from SNR. The average pore diameter, however, practically remains same (~ 40 Ǻ) in all three samples. The XRD of air-dried SN, SNR and WSNR are given in Fig. 1. It is seen that SN is mostly amorphous in nature with a few low intensity peaks corresponding mainly to quartz todorokite. After reduction roasting followed by leaching, the XRD peaks due to todorokite disappear because of its consumption in the formation of metal, especially Mn silicates. In addition, formation of MnCO 3 is also evident from the appearance of its characteristic peaks in SNR. On washing with distilled water, no change in the characteristic peak positions is observed from that of SNR. On calcinations the intensity of characteristic peaks of MnCO 3 decreases due to its decomposition and almost disappears at around 500 C. FTIR spectra of air-dried SN, SNR and WSNR (untreated and heat treated) revealed that broad absorption band at ~3445 cm -1 and moderately intense band at ~1650 cm -1 are attributed to O-H stretching and bending modes of vibrations 31. On washing the SNR with distilled water, the position of majority bands remain same, except the disappearance of absorption band at 1072 cm -1, presumably due to loss of small amount of loosely bound NH 3 or sulphate on washing 32. The sulphate is most likely generated from the impurities of coal during reduction roasting with sea nodules. Oxidative decolourization of Rhodamine-B Effect of dye concentration The effect of initial Rhodamine-B concentration on decolourization by SNR has been studied (Fig. 2) taking nodule loading of 0.5 g/l at initial ph 3.0. The concentration of Rhodamine-B ranges from 5 to 30 mg/l. At the concentration (5 mg/l) the decolourization percentage reaches to 93% within 1 h. However, the percentage of decolourization decreases by increasing concentration of Rhodamine-B. It is well established that oxidative degradation of organic matter by Mn-oxides occurs on the surface of the catalyst 2,7, not in the aqueous phase. The organic compounds are adsorbed on the surface to form the

3 SATAPATHY et al.: OXIDATIVE DECOLOURIZATION OF RHODAMINE-B 259 Fig.1 Powder X-ray diffraction of sea nodule (SN), sea nodule residue (SNR), washed sea nodule residue (WSNR) and WSNR heated at 400 C Fig.2 Effect of initial concentration of Rh-B on decolourization surface precursor complex and then electron transfer takes place from organic compound to the surface bound Mn (III)/(IV), followed by release of oxidation product as soluble Mn (II). Figure 2 shows that at a fixed loading of the sea nodule residues, decolourization decreases with increasing initial concentration. This indicates that reactive surface sites are saturated and do not provide active sites for further formation of precursor complex. Thus, percentage of decolourization decreases at higher Rhodamine-B concentration. The experimental Fig.3 Effect of catalyst loading on decolourization of Rhodamine-B findings suggest that surface reactivity and number of absorption sites are two crucial factors for oxidative decolourization of Rhodamine-B. Catalyst loading The effect of catalyst loading on decolourization of Rhodamine-B by SNR is also studied (Fig. 3) taking Rhodamine-B concentration 10 mg/l at initial ph 3.0. The catalyst loading varies from 0.2g/L to 1.0 g/l. At the catalyst loading of 0.2g/L the decolourization percentage is less. However, by increasing catalyst loading the decolourization percentage increases and

4 260 INDIAN J. CHEM. TECHNOL., JULY 2014 sorption sites. Hence, further adsorption and oxidation of dye compound on the catalyst particle are greatly inhibited 17. Present study indicates that lower ph of the suspension suppressed Rhodamine-B adsorption on the SNR but increases reduction potential of Mn (hydro) oxide/mn 2+ couple and enhances decolourization of Rhodamine-B. Fig.4 Effect of initial ph on decolourization of Rhodamine-B becomes 96% for catalyst loading 1g/L. It is due to increase of surface active sites by increasing catalyst loading from 0.2g/L to 1g/L. Initial ph The decolourization of Rhodamine-B at various ph ( ) as a function of reaction time is shown in Fig. 4. The decolourization rate of dye compound decreases with increasing ph. At ph 3, 65% of decolourization takes place within 1 h whereas this value decreases slightly for higher ph. This decrease in activity with increase in ph may be described as follows. The oxidation of organic dye on manganese nodule suspension appears to be a heterogeneous reaction, which involves the diffusion of dye compound onto the catalyst surface to form surface precursor complex between the reactants, followed by electron transfer and products release 9. The surface charge of sea nodule residue plays a vital role in the formation of surface complex. The zero point charge (ph pzc ) of washed sea nodule residue (WSNR) is determined to be 6.5. At lower ph than the ph pzc (6.5) the surface of the residue is positively charged due to protonation, which does not favour cationic dye (Rhodamine-B as model dye) adsorption and hinders the formation of surface precursor complex due to electrostatic repulsion. On the other hand, at higher suspension ph (>6.5) the surface is negatively charged due to deprotonation, favors surface complex formation. Though lower ph inhibits the surface complex formation, it improves reduction potential of Mn (hydro) oxide/mn 2+ couple. In contrast, the increase in suspension ph decreases oxidizing power of Mn (hydro) oxides and favors the adsorption of Mn (II) on the SNR surfaces, resulting in decreasing surface Conclusion Sea nodule residue exhibit good catalytic activity for oxidative decolourization of Rhodamine-B. The decolourization activity decreases with the increase in ph and initial Rh-B concentration, however the decolourization percentage of Rh-B increases with increase in the catalyst dose. More than 93% decolourisation of Rh-B with initial concentration 5 mg/l is achieved within 1 h at ph 3.0 and catalyst dose 0.5 g/l. References 1 Parida K M, Satapathy P K & Das N N, J Colloid Interface Sci,181 (1996) Bhattacharjee S, Chakrabarty S, Maity S, Kar S, Thakur K & Bhattacharyya G, Water Res, 37 (2003) Kumari A & Natarajan K A, Hydrometallurgy, 64 (2002) Parida K M & Mohanty S, J Colloid Interface Sci, 199 (1998) Parida K M, Gorai B & Das N N, J Colloid Interface Sci, 187 (1997) Liu R & Tang H, Water Res, 34 (2000) Zhu M X, Wang Z & Zhou LY, J Hazard Mater, 150 (2008) Gemeay A H, El-Sharkawy R G, Mansour I A & Zaki A B, Appl Catal B: Environ, 80 (2008) Zhang W, Yang Z, Wang X, Zhang Y, Wen X & Yang S, Catal Commun, 7 (2006) Parida K M, Satapathy P K & Das N N, J Colloid Interface Sci, 173 (1995) Parida K M, Mallick S & Dash S S, J Colloid Interface Sci, 290 (2005) Parida K M & Pradhan A C, J Hazard Mater, 173 (2010) Parida K M, Mallick S, Mohapatra B K & Mishra V N, J Colloid Interface Sci, 277 (2004) Dash S S & Parida K M, J Colloid Interface Sci,. 307 (2007) Parida K M, Sahu S, Reddy K H & Sahoo P C, Ind Eng Chem. Res. 50 (2011) Mallick S, Dash S S & Parida K M, J. Colloid Interface Sci, 297 (2006) Satapathy P K, Randhawa N S & Das N N, Environ Technol, 33 (2012) Satapathy P K, Acharya B & Das N N, Indian J Chem Technol, 18 (2011) Agrawal A, Sahu K K & Pandey B D, Colloids Surf A, 237 (2004) Das N N & Jana R K, J Colloid Interface Sci, 293 (2006) Behera R K, Satapathy P K, Randhawa N S & Das N N, Adsorp Sci Technol, 28 (2010) 611.

5 SATAPATHY et al.: OXIDATIVE DECOLOURIZATION OF RHODAMINE-B Agrawal A & Sahu K K, J Hazard Mater B, 137 (2006) Gulnaz O, Kaya A, Matyar F & Arikan B, J Hazard Mater,108 (2004) Zhao M, Tang Z & Liu P, J Hazard Mater, 158 (2008) Gupta V K & Ali I, Encyclopaedia of Surface and Colloid Science, edited by Hubbard (Marcel Dekker, New York), Vol 1, 2002, Nogueira F G E, Lopes J H, Silva A C, Gonçalves M, Anastacio A S, Sapag K & Oliveira L C A, Appl Clay Sci, 43 (2009) Kuo W G, Water Res, 26 (1992) Davis A P & Huang C P, Water Res, 24 (1990) Liu R & Tang H, Water Res, 34 (2000) Maity S, Chakravarty S, Bhattacharjee S & Ray B C, Water Res, 39 (2005) Jana R K, Srikanth S, Pandey B D, Kumar V & Premchand, Met Mater Processes, 11 (1999) Piper D Z, Baster J R & Bischoff J L, Geochim Cosmochim Acta, 48 (1984) 2347.

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