Methylene blue adsorption by pyrolytic tyre char
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1 NATIONAL UNIVERSITY OF SINGAPORE Division of Environmental Science and Engineering Division of Environmental Science and Engineering EG2605 UROP Report Methylene blue adsorption by pyrolytic tyre char Professor: Dr Rajasekhar Bala Yeo Kai Yun U065998Y Duration of experiment: 19/05/ /07/2008 EG2605 report Page 1
2 ABSTRACT Activated carbons produced from waste tyre rubber have shown exceptional characteristics for the adsorption of organic species from solution. The purpose of this experiment is to investigate the adsorption of methylene blue, with various parameters, on pyrolytic tyre char at room temperature. In studying its aqueous adsorption characteristics using methylene blue, adsorption data were modeled to the Langmuir equation in order to determine the adsorption capacities (Xm) and affinity parameter (Ka). The rates of adsorption were found to conform to the pseudo-second-order kinetics. Also, ph variations were made and concluded that ph values of 5-7 gave higher adsorption capacities. SEM photos showed the differences between activated and un-activated carbon and the effects on adsorption of methylene blue. 1. INTRODUCTION The objective of this study was to assess the ability of activated carbon derived from used rubber tyres to remove an organic dye, methylene blue, from aqueous solution. We also investigated the kinetics, ph effects, adsorbate concentrations and ratios of adsorbent to adsorbate. The char preparation process involves heating rubber tyres to 550 degrees Celsius for pyrolysis. After pyrolysis, as temperature cools, we introduced oxygen. When temperature reaches 250 degree Celsius, we stopped the oxygen flow. This results in the decomposition of the rubber polymer and the formation of a hydrocarbon oil, a high calorific gas and a carbonized char (1,6). The oil has been suggested for use as a fuel or as a source of refined chemicals, while the pyrolysis gas can be recycled on-site to self-fuel the process. Such rubber-derived carbons have low mechanical strength and are produced in powdered form, making them best suited for use in liquid phase applications. The presence of zinc in the rubber tyres has potential for exploration. Although rubber derived carbons may not be suited for high purity treatments, they are adequate for treatment of industrial or domestic effluents. Little work has been produced on the aqueous adsorption characteristics of activated carbons produced from waste tyre rubber. (C. J. Sollars et al., 2002) 2. MATERIALS AND METHODS 2.1 Materials Adsorbent: Waste rubber tyre (final particle size is between 45µm and 150 µm.) Adsorbate: Methylene Blue (82% purity, g/mol) Reagents: Purified water from a Milli-Q water system from Millipore, USA 2.2 Analytical method Instrument 0.1g of activated carbon was added to 100ml of methylene blue solution at varying concentrations diluted with distilled water. Solutions all shaken for 14 hours at 150 rpm. The solution and solid phase were separated by filtration with Whatman number 4 filter paper. More than 4ml aliquot of the supernatant was removed and analysed. The UV-VIS spectrophotometer (U-2800) was used to measure absorbance. Adsorption capacity was then calculated Experimental techniques and procedure The methylene blue concentration was determined in a U-2800 UV VIS spectrophotometer by measuring the light absorbance at a wavelength of 665 nm. Adsorption tests were carried out in 3 stages. Firstly, for the calculation of isotherms at 25 C, different conical flasks containing 0.1 g of activated carbon and 100mL of solution were shaken for 14 hours. Different initial adsorbate concentrations were used: 10, 20, 25, 40, 50, 60, 75, 80, 100, 200, 300, 400 and 500 mg/l. The amount of adsorbate retained in equilibrium (qe) was then calculated. Next, the kinetics of the adsorbent was studied. 0.1 g of the corresponding adsorbent was EG2605 report Page 2
3 placed in 100mL of an initial methylene blue concentration (C0) of 500 mg/l The residual concentration of methylene blue in solution, C (mg/l) was measured after 1, 5, 10, 15, 30, 60, 120, 180, 240, 300 and 360 min. By equilibrium of masses, the adsorption q (mg/g), was found for each time. Second-order kinetics is expressed by the integrated and linearized equation, where K2 (g/mg min) is the kinetic constant. Finally, effects of different ph on the adsorption capacity were studied with ph 3,4,5,6 and g of activated carbon was mixed with 100mg of methylene blue solution for each ph. 3. RESULTS AND DISCUSSION 3.1 Adsorption isotherms 3.1a Experimenting with un-activated carbon From previous results, 300ppm and 200ppm give more reliable readings hence this experiment would only comprise 300ppm and 200ppm of MB. Table of absorbance for 200ppm and 300ppm MB a B Control At 200ppm Average At 300ppm Average Calculations From calibration graph y = 19.71x, Concentration = (1.071)(19.71) = Since we diluted 5 times, actual concentration = x 5 = mg/l Ce = mg/l Concentration for control = x x 5 = mg/l Sorption = = mg/l q for 100mL of solution = amount of contaminant adsorbed/ mass of adsorbant = ( /10)mg / g = mg/g Ce/q = / = EG2605 report Page 3
4 Ka=0.1933/0.197= L/mg (affinity between methylene blue and char) Xm=1/0.1933= mg/g (maximum adsorption capacity of char) Discussion Langmuir s equation : Ce/qe= Ce/Xm + 1/KaXm is based on a theoretical model and supposes that maximum adsorption consists in a saturated monolayer of molecules of adsorbate on the surface of the adsorbent, considered energetically homogenous from the point of view of adsorption, where qe (mg/g) is adsorption capacity at equilibrium, Ce (mg/l) the concentration in the liquid phase at equilibrium, Xm (mg/g) the maximum adsorption capacity per unit of mass necessary for the formation of a complete monolayer on the surface and Ka (L/mg) is a constant related with affinity for the adsorption sites. The linear graph of Ce/qe versus Ce shows that adsorption follows the Langmuir isothermal model, indicating the homogeneous nature of pyrolytic char surface, i.e., each methylene blue molecule/char adsorption has equal adsorption activation energy; the results also demonstrate the formation of a single layered coverage of dye molecule at the outer char surface. The steep slope of the Langmuir plots shows the usefulness of pyrolytic char at high concentration its efficiency in column operations. As the concentration of the solution increased, adsorption occurred more readily due to a synergistic effect, with the adsorbed molecules facilitating the adsorption of more molecules as a result of adsorbate-adsorbate interactions. This was especially so for methylene blue, having a relatively large hydrophobic component. (V. Gomez, 2007) For values of the adsorption parameters, comparing with earlier studies done, our maximum adsorption capacity of activated char is lower. In the journal published by F. Rozada et al., activated carbon obtained from pyrolysed tyres could yield an Xm value of 41.0 mg/g and Christopher Sollars et al. yielded a minimum value of 74mg/g. The difference can also be attributed to the different activation conditions from us. However, our affinity constant is much higher at L/mg compared to 0.08 L/mg reported by F. Rozada et al.. EG2605 report Page 4
5 3.1b Experimenting with varying ratios of MB solution (ml): mass of activated carbon (mg) Discussion From the first graph, for 100ppm methylene blue solution, the amount of activated carbon for optimal adsorption per unit mass of activated carbon is 0.08g. However, the second graph indicates that the mass of adsorbent for optimal overall removal of methylene blue is 0.1g. As we are interested in the overall removal, we selected 0.1g of activated carbon for the proceeding experiment on kinetics. The graph also shows the varying degree of effectiveness of adsorbent to adsorbate ratio. For 100mL of methylene blue and 0.05g of activated carbon, the removal was slightly more than half. From 0.1 to 0.2g of activated carbon per 100mL methylene blue solution, the removal was 100%. EG2605 report Page 5
6 3.2 Adsorption kinetics Experiment at 100ppm MB solution with activated char Discussion From the graph, there is an increase in percentage removal of methylene blue by activated carbon and this percentage increases with time. The first 30 minutes show the highest rate of adsorption, afterwhich the rate decreases to almost a constant by 210 minutes. The time profile of dye uptake is a smooth and continuous curve that plateaus off at saturation, suggesting also the possible monolayer coverage of dyes on the surface of the char. We can fit the experimental data to a second order equation, giving us a correlation of , k value of and Ce value of 36 mg/l. Kinetic data can be further treated with the pseudo-second order kinetic model with the following the differential equation: dqt/dt = k2(qe qt)2 where k2 is the equilibrium rate constant of pseudo-secondorder adsorption (g/ mg /min). Integrating it for the boundary condition t = 0 to t and qt = 0 to qt, gives: 1/(qe qt)= 1/qe + k2t which is the integrated rate law for a pseudo-second-order reaction. It can be rearranged to obtain a linear form: t/qt =1/k2qe2 +1/qet If pseudo-second-order kinetics is applicable, the plot of t/qt versus t should show a linear relationship. The linear plots of t/qt versus t show a good agreement of experimental data with the pseudo-second-order kinetic model for both The calculated qe values agree very well with the experimental data These indicate that the adsorption of direct dyes from wastewater on char obeys pseudo-second-order kinetic model (Malik, 2004). 3.3 Effects of ph on adsorption EG2605 report Page 6
7 Discussion The ph of the system influences the adsorptive uptake of adsorbate molecule presumably due to its influence on the surface properties of the adsorbent and ionization/dissociation of the adsorbate molecule. The variations in removal of methylene blue at various system ph are shown in the above graph. From the graph, the maximum removal of methylene blue for both the samples is above Un-activated carbon experiments Comparison of amount of methylene blue sorped in 20ppm solution using activated and unactivated carbon The amount sorped was generally higher for activated carbon Comparison of % removal of methylene blue in 20ppm solution using activated and un-activated carbon From the above graph, it is obvious that the activated carbon is more effective in removing methylene blue from aqueous solution, reaching almost full removal compared to un-activated carbon, which reached about 70% removal. EG2605 report Page 7
8 Comparison of kinetics of methylene blue in 50ppm solution using activated and un-activated carbon From the above graphs, it is clear that activated char is more effective in removing methylene blue, reaching 50-60% removal while unactivated char only reached around 10% removal. The rate of reaction for activated char was also faster than unactivated char. 3.6 Scanning Electron Microscope results Un-activated char at 1000x magnification EG2605 report Page 8
9 Un-activated char at 100x magnification Activated char at 5000x magnification A crack can be seen, a result of activating the carbon. Methylene blue coated on activated char at 1000x magnification Pores around 20 micro metre in width are visible, giving rise to better adsorption of methylene blue. EG2605 report Page 9
10 4. CONCLUSION Activated carbons produced from tyre rubber exhibited exceptional characteristics for the adsorption of organic compounds from solution. Activation resulted in a significant development in the carbon porosity, which was reflected in greater capacities for the adsorption of organic compounds from solution. This study concludes that activated carbon prepared from waste material, rubber tyre, is considerably efficient for adsorption of dyes. The adsorption is highly dependent on contact time, adsorbent concentration and ph. The most ideal ph for adsorption of methylene blue on the char is ph values of 5-7. The kinetics of methylene blue adsorption on pyrolytic char follows the pseudo-secondorder model. The equilibrium data fit well in the Langmuir model of adsorption, showing monolayer coverage of dye molecules at the outer surface of the char. The value for the maximum adsorption capacity, Xm, is lower than the values for commercial activated carbon reported in earlier studies, but affinity constant, Ka, is higher. 5. ACKNOWLEDGEMENTS I would like to thank Dr R. Bala for the opportunity to participate in UROP and Augustine Quek for his guidance. 6. REFERENCES A study of the characteristics of activated carbons produced by steam and carbon dioxide activation of waste tyre rubber. Guillermo San Miguel, Geoffrey D. Fowler, Christopher J. Sollars. Centre for Environmental Control and Waste Management, Department of Civil and Environmental Engineering, Imperial College of Science, Technology and Medicine, London SW7 2BU, UK. Carbon 41 (2003) Adsorption. Retrieved 8 July 2008 from Environ/Adsorb/adsorb.htm Activated carbons from sewage sludge and discarded tyres: Production and optimization F. Rozada, M. Otero, A. Mor an, A.I. Garc ıa. Department of Chemical Engineering, IRENA-ESTIA, Natural Resources Institute, University of Le on, Avda. Portugal 41, Le on, Spain Received 1 February 2005; received in revised form 3 May 2005; accepted 4 May Journal of Hazardous Materials B124 (2005) Adsorption of organic compounds from solution by activated carbons produced from waste tyre rubber. G. San Miguel, G. D. Fowler, and C. J. Sollars. Department of Civil and Environmental Engineering, Centre for Environmental Control and Waste Management, Imperial College of Science, Technology and Medicine, London SW7 2BU, UK. Separation Science and technology, 37(3), (2002). Application in fixed-bed systems of adsorbents obtained from sewage sludge and discarded tyres F. Rozada, M. Otero, A.I. Garcı a, A. Mora n. Department of Chemical Engineering, IRENA-ESTIA, Natural Resources Institute, University of Leo n, Avda. Portugal 41, Leo n, Spain Received 28 April 2005; received in revised form 17 June 2005; accepted 12 July 2005 Dyes and Pigments 72 (2007) 47e56 Dye removal from wastewater using activated carbon developed from sawdust: adsorption equilibrium and kinetics. P.K. Malik. Department of Chemistry, Centre for Surface Science, Jadavpur University, Kolkata 32, India. Received 8 April 2003; received in revised form 20 April 2004; accepted 17 May Journal of Hazardous Materials B113 (2004) EG2605 report Page 10
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