Faculty Publications
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Item Synthesis and antimicrobial activities of some novel 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles and 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazines carrying thioalkyl and sulphonyl phenoxy moieties(2007) Karabasanagouda, T.; Vasudeva Adhikari, A.V.; Shetty, N.S.Thirty one new 6-aryl-3-{(4-substituted phenoxy) methyl}-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles (6a-s) and 6-aryl-3-{(4-substituted phenoxy methyl}-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazines (7a-l) have been synthesized from 4-thioalkyl phenols (1a-b) through a multi-step reaction sequence. Compounds 1a-b reacted with ethyl chloroacetate in presence of acetone and potassium carbonate to give ethyl [4-(thioalkyl) phenoxy] acetates (2a-b). Further, 2a was oxidized to [4-(methyl sulphonyl) phenoxy] acetate (2c) using hydrogen peroxide in acetic acid. Reactions of (2a-c) with hydrazine hydrate in alcoholic medium furnished 2-[4-thiosubstituted phenoxy] acetohydrazides (3a-b) and 2-[4-methyl sulphonyl phenoxy] acetohydrazide (3c) which on treatment with carbon disulphide and methanolic potassium hydroxide yielded corresponding potassium dithiocarbazates (4a-c). They were then converted to 4-amino-5-{(4-thioalkyl phenoxy) methyl}-4H-1,2,4-triazole-3-thiols (5a-b) and 4-amino-5-{(4-methyl sulphonyl phenoxy) methyl}-4H-1,2,4-triazole-3-thiol (5c) by refluxing them with aqueous hydrazine hydrate. The title compounds 6a-s were prepared by condensing 5a-c with various aromatic carboxylic acids in presence of phosphorus oxychloride. The intermediates 5a-c, on condensation with various substituted phenacyl bromides afforded a series of title compounds (7a-l). The structures of new compounds 2a-7l were established on the basis of their elemental analysis, IR, 1H NMR, 13C NMR and mass spectral data. All the title compounds were subjected to in vitro antibacterial testing against four pathogenic strains and antifungal screening against three fungi. Preliminary results indicate that some of them exhibited promising activities and they deserve more consideration as potential antimicrobials. © 2006 Elsevier Masson SAS. All rights reserved.Item An optimization study on microwave irradiated, decomposition of phenol in the presence of H2O2(2009) Prasannakumar, B.R.; Iyyaswami, I.; Murugesan, T.Background: Removal of phenol from industrial waste waters involves basic techniques namely extraction, biodegradation, photocatalytic degradation, etc. Among the available processes, the oxidation of phenols using H2O2 is a suitable alternative because of low cost and high oxidizing power. The application of an oxidation process for the decomposition of stable organic compounds in waste water leads to the total degradation of the compounds rather than transferring from one form to another. Since oxidation using Fenton's reagent ismore dependent on pH, in this present work it was proposed to use H2O2 coupled with microwave irradiation. The effects of initial phenol concentration, microwave power and the irradiation time on the amount of decomposition were studied. Results: In the present work experiments were conducted to estimate the percentage degradation of phenol for different initial concentrations of phenol (100, 200, 300, 400 and 500 mg L-1), microwave power input (180, 360, 540, 720 and 900 W) for different irradiation times. The kinetics of the degradation process were examined through experimental data and the decomposition rate follows first-order kinetics. Response surface methodology (RSM) was employed to optimize the design parameters for the present process. The interaction effect between the variables and the effect of interaction on to the responses (percentage decomposition of phenol) of the process was analysed and discussed in detail. The optimum values for the design parameters of the process were evaluated (initial phenol concentration 300 mg L-1, microwave power output 668 W, and microwave irradiation time 60 s, giving phenol degradation 82.39%) through RSM by differential approximation, and were confirmed by experiment. Conclusion: The decomposition of phenol was carried out using H2O2 coupled with microwave irradiation for different initial phenol concentrations, microwave power input and irradiation times. The phenol degradation process follows first-order kinetics. Optimization of the process was carried out through RSM by forming a design matrix using CCD. The optimized conditions were validated using experiments. The information is of value for the scale up of the oxidation process for the removal of phenol from wastewater. © 2008 Society of Chemical Industry.Item Effective oxidation of alcohols by Iron(III)-Schiff base-triphenylphosphine complexes(2010) Rani, S.; Badekai Ramachandra, B.Iron(III)-Schiff base-triphenylphosphine complexes catalyze the oxidation of alcohols to their corresponding carbonyl compounds in presence of hydrogen peroxide in good yields. © 2010 Elsevier Ltd. All rights reserved.Item Enhanced degradation of paracetamol by UV-C supported photo-Fenton process over Fenton oxidation(2011) Manu, B.; Mahamood, S.For the treatment of paracetamol in water, the UV-C Fenton oxidation process and classic Fenton oxidation have been found to be the most effective. Paracetamol reduction and chemical oxygen demand (COD) removal are measured as the objective functions to be maximized. The experimental conditions of the degradation of paracetamol are optimized by the Fenton process. Influent pH 3, initial H 2O 2 dosage 60 mg/L, [H 2O 2]/[Fe 2+] ratio 60 : 1 are the optimum conditions observed for 20 mg/L initial paracetamol concentration. At the optimum conditions, for 20 mg/L of initial paracetamol concentration, 82% paracetamol reduction and 68% COD removal by Fenton oxidation, and 91% paracetamol reduction and 82% COD removal by UV-C Fenton process are observed in a 120 min reaction time. By HPLC analysis, 100% removal of paracetamol is observed at the above optimum conditions for the Fenton process in 240 min and for the UV-C photo-Fenton process in 120 min. The methods are effective and they may be used in the paracetamol industry. © IWA Publishing 2011.Item Solar photocatalysis for treatment of Acid Yellow-17 (AY-17) dye contaminated water using Ag@TiO2 core-shell structured nanoparticles(2013) Khanna, A.; Shetty K, K.Wastewater released from textile industries causes water pollution, and it needs to be treated before discharge to the environment by cost effective technologies. Solar photocatalysis is a promising technology for the treatment of dye wastewater. The Ag@TiO2 nanoparticles comprising of Ag core and TiO2 shell (Ag@TiO2) have unique photocatalytic property of inhibition of electron-hole recombination and visible light absorption, which makes it a promising photocatalyst for use in solar photocatalysis and with higher photocatalytic rate. Therefore, in the present work, the Ag@TiO2 nanoparticles synthesized by one pot method with postcalcination step has been used for the degradation of Acid Yellow-17 (AY-17) dye under solar light irradiation. The Ag@TiO2 nanoparticles were characterized using thermogravimetric-differential thermal analysis, X-ray diffraction, transmission electron microscopy, selected area electron diffraction, and energy dispersive X-ray analysis. The catalyst has been found to be very effective in solar photocatalysis of AY-17, as compared to other catalysts. The effects of pH, catalyst loading, initial dye concentration, and oxidants on photocatalysis were also studied. The optimized parameters for degradation of AY-17 using Ag@TiO2 were found to be pH 3, dye/catalyst ratio of 1:10 (g/g), and 2 g/L of (NH4)2S2O8 as oxidant. Efficient decolorization and mineralization of AY-17 was achieved. The kinetics of color, total organic carbon, and chemical oxygen demand removal followed the Langmuir-Hinshelwood model. Ag@TiO2 catalyst can be reused thrice without much decline in efficiency. The catalyst exhibited its potential as economic photocatalyst for treatment of dye wastewater. © 2013 Springer-Verlag Berlin Heidelberg.Item Novel one-pot green synthesis of graphene in aqueous medium under microwave irradiation using a regenerative catalyst and the study of its electrochemical properties(Royal Society of Chemistry, 2015) Subramanya, B.; Bhat, D.In this work we report an economic, eco-friendly, high yielding and facile one-pot method for the large scale synthesis of few layer graphene (FLG) nanosheets directly from graphite in aqueous medium using a regenerative catalyst, sodium tungstate. This method is fast and makes use of environmental friendly chemicals and microwave radiation. The as-synthesized FLG nanosheets are characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and Brunauer-Emmett-Teller (BET) surface area analysis. Raman analysis indicates that the as-synthesized graphene is bilayered with a smaller domain size of 3.9 nm which is responsible for a higher specific surface area of FLG nanosheets (1103.62 m2 g-1). Moreover, XPS analysis of FLG nanosheets shows a high C:O ratio (?9.6) which is the best among the graphene prepared from green chemicals. The electrochemical performance of as-synthesized FLG nanosheets is analysed by cyclic voltammetry (CV), chronopotentiometry and electrochemical impedance spectroscopy (EIS) in neat 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIMBF4) electrolyte. The superior capacitive performance with large capacitance (219 F g-1), high energy density (83.56 W h kg-1) and excellent cyclability (3000 cycles) exhibited by these graphene nanosheets make them an excellent candidate for supercapacitor material. © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015.Item Nano Fe3O4@APTES@Ni(OH)2 as a catalyst for alcohol oxidation(Royal Society of Chemistry, 2015) Bhat, P.B.; Badekai Ramachandra, B.R.A nanorod shaped nickel hydroxide coated ferrite nanocatalyst was synthesized by a traditional co-precipitation method. The particle size of the nanoferrite was tuned using a variable surfactant ratio to achieve a high surface area. A very high BET surface area (334.55 m2 g-1) was achieved for particles with sizes of 40-130 nm. The superparamagnetic reusable catalyst was found to be active for the selective liquid phase oxidation of alcohols with hydrogen peroxide as a mild oxidant. Nickel hydroxide acted as a Bronsted base working in synergy with the nanoferrite catalyst for alcohol oxidation. The catalytic system was found to catalyse primary and secondary alcohols efficiently (86%) to their corresponding carbonyls in good yields. © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015.Item Low cost Fenton's oxidative degradation of 4-nitroaniline using iron from laterite(IWA Publishing 12 Caxton Street London SW1H 0QS, 2016) Amritha, A.S.; Manu, B.The present study aims to establish the use of iron (Fe) from larerite in the case of Fenton's oxidation process which is a simple and cost-effective method for degradation of nitro compounds in effluents and in surface or ground water. 4-nitroaniline (4-NA) degradation by Fenton's oxidation method is the subject of the present study so as to optimize pH, hydrogen peroxide/iron (H/F) ratio at different initial concentrations of 4-NA. The optimum pH obtained was 3. The present study has also established optimum H/F ratio for the different initial concentrations of 4-NA for both conventional and use of Fe from laterite. The maximum removal efficiency of 99.84% was obtained for an H/F ratio of 100 for 0.5 mM initial concentration of 4-NA. The study establishes the use of Fe extracted from locally available laterite soil (LS) as a replacement of Fe salts so as to reduce the cost of the process. © 2016 IWA Publishing.Item Fenton's treatment of actual agriculture runoff water containing herbicides(IWA Publishing 12 Caxton Street London SW1H 0QS, 2017) Sangami, S.; Manu, B.This research was to study the efficiency of the Fenton's treatment process for the removal of three herbicides, namely 2,4-dichlorophenoxy acetic acid (2,4-D), ametryn and dicamba from the sugarcane field runoff water. The treatment process was designed with the Taguchi approach by varying the four factors such as H 2 O 2 /COD (1-3.5), H 2 O 2 /Fe 2+ (5-50), pH (2-5) and reaction time (30-240 min) as independent variables. Influence of these parameters on chemical oxygen demand (COD), ametryn, dicamba and 2,4-D removal efficiencies (dependent variables) were investigated by performing signal to noise ratio and other statistical analysis. The optimum conditions were found to be H 2 O 2 /COD: 2.125, H 2 O 2 /Fe 2+ : 27.5, pH: 3.5 and reaction time of 135 min for removal efficiencies of 100% for ametryn, 95.42% for dicamba, 88.2% for 2,4-D and with 75% of overall COD removal efficiencies. However, the percentage contribution of H 2 O 2 /COD ratio was observed to be significant among all four independent variables and were 44.16%, 67.57%, 51.85% and 50.66% for %COD, ametryn, dicamba and 2,4-D removal efficiencies, respectively. The maximum removal of herbicides was observed with the H 2 O 2 dosage of 5.44 mM and Fe 2+ dosage of 0.12 mM at pH 3.5. © IWA Publishing 2017 W.Item rGO/MnO2 nanowires for ultrasonic-combined Fenton assisted efficient degradation of Reactive Black 5(IWA Publishing 12 Caxton Street London SW1H 0QS, 2017) Ramesh, M.; Rao, M.P.; Rossignol, F.; Nagaraja, H.S.Reduced graphene oxide (rGO) coated manganese dioxide (MnO2) nanowires (NWs) were prepared by the hydrothermal method. Raman spectra confirmed the presence of rGO and the Brunauer-Emmett-Teller surface area of rGO/MnO2 NWs was found to be 59.1 m2g-1. The physico-chemical properties of prepared catalysts for the degradation of Reactive Black 5 (RB5) dye were investigated. 84% of RB5 dye in hydrogen peroxide solution was successfully degraded using rGO/MnO2 NWs, while only 63% was successfully degraded with pristine ?-MnO2 NWs in 60 min owing to the smaller crystallite size and large surface area. Further, the ultrasonic-combined Fenton process significantly enhanced the degradation rate to 95% of RB5 by the catalyst rGO/MnO2 NWs due to synergistic effects. The decomposition products identified using gas chromatography-mass spectrometry revealed a higher production rate of fragments in the ultrasonic-combined Fenton process. Therefore, rGO/MnO2 NWs with the ultrasonic-combined Fenton process is an efficient catalyst for the degradation of RB5, and may be used for environmental protection. © IWA Publishing 2017.
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