Ntcc report final report shubham

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  1. 1. Synthesis of Magnetic Cryptomelane-type manganese oxide (OMS-2) nanotubes for the removal of lead based compounds from water samples Submitted to Amity Institute of Nanotechnology Amity University, Noida In partial fulfillment of the requirements for the degree of B.TECH+M.TECH NANOTECHNOLOGY By: Shubham Raina ENROLLMENT NO.: A1223313003 Under the guidance of Dr. Ranjit Kumar
  2. 2. 2 AMITY INSTITUTE OF NANOTECHNOLOGY PROJECT REPORT-2015 PROJECT TITLE : Synthesis of Magnetic Cryptomelane-type manganese oxide (OMS-2) nanotubes for the removal of lead based compounds from water samples PROGRAMME : B.tech+ M.techNanotechnology SEMESTER : 5 NAME of STUDENT : Shubham Raina ENROLLMENT NO : A1223313003 BATCH : 2013-2018 DURATION : 30 days NAME OF GUIDE : Dr. Ranjit Kumar Internal Guide Student
  3. 3. 3 DECLARATION BY THE CANDIADTE I hereby declare that the matter in the project report entitled Synthesis of Magnetic Cryptomelane-type manganese oxide (OMS-2) nanotubes for the removal of lead basedcompounds from water samples submitted to Dr. Ranjit Kumar , AssistantProfessor, Amity Institute of Nanotechnology, Amity University, and Noida is a bonafide and genuine research project under the guidance of Dr. Ranjit Kumar. The work done in the report is original and has not been submitted earlier for the award of any degree, diploma, or fellowship of any other university or institution. Date: July 15, 2015 NAME : Shubham Raina Enrolment no. : A1223313003
  4. 4. 4 CERTIFICATE BY THE GUIDE This is to certify that the report entitled Synthesis of Magnetic Cryptomelane-type manganese oxide (OMS-2)nanotubes for the removal of lead basedcompounds from watersamples is a bonafide research work carried out by Shubham Raina, which is submitted in partial fulfillment for the award of the degree of B.tech + M.tech Nanotechnology in the Amity University, Noida . Date: Prof. Dr. Ranjit Kumar Place: Noida, Uttar Pradesh
  5. 5. 5 ACKNOWLEDGEMENT I would like to thank Dr. Ranjit Kumar for giving me such interesting and challenging topic to carry out my experimental research project . I would also like to thank sir for helping me , guiding me by providing relevant and important concepts and other important data regarding my experimental work .
  6. 6. 6 Table of contents S.No. Topic Page no. 1. ABSTRACT PAGE 8 2. INTRODUCTION Page 8 3. EXPERIMENTAL PROTOCOL Page 9 4. SAMPLE CHARACTERIZATION Page 10 5. RESULTS AND DISCUSSION Page 11 6. FUTURE WORK Page 12
  7. 7. 7 7.. CONCLUSION Page 12 8. REFERENCES Page 13
  8. 8. 8 Abstract Magnetic cryptomelane-type manganese oxide nanotubes were successfully prepared by depositing Iron(II) oxide (magnetite/ Fe3O4) nanoparticles onto the nanotubes. The synthesized material exhibits excellent magnetic and catalytic properties for the degradation of lead based compounds fromwater samples and can be magnetically separated from the solution with ease leaving clear water behind . Introduction Manganese oxide is a type of microporous transition metal oxide that can form mixed-valent semiconducting octahedral molecular sieves (OMS) with tunnel like structures of various sizes [2]. OMS materials have extensive applications and advantages such as low cost, high adsorption activity, and non-toxicity [310]. Among these, -MnO2 (cryptomelane, OMS-2), having an ordered tunnel structure shared with MnO6 octahedral chains, has been extensively used as a cathode material [11],adsorbents [8,13], and catalysts [1417]. OMS-2 nanotubes can be easily prepared by hydrothermal treatment of KMnO4 in the HCl solution [5, 8, 17] and has been recently revealed to possesshigh adsorption capability for dye degradation and heavy metal ion removal in wastewaters [13, 16]. In most research reports it remains a challenge to develop a simplistic and economic rout to separation or recovery of these nano- materials from heterogeneous systems. To solve this problem magnetic separation is being considered an ideal alternative to the removal of in situ nanomaterials via magnetic induction [13]. In this report the successfulsynthesis of ferromagnetic cryptomelane-type nanotubes have been carried out by a combination of hydrothermal and precipitation techniques, and the prepared Fe3O4-OMS-2 nanotube compositeexhibited excellent adsorption efficiency for the degradation of lead based compounds from water samples .
  9. 9. 9 Experimental Protocol Preparationof OMS-2 Nanotubes To synthesize MnO2 nanotubes, a hydrothermal method was carried out [17]. 0.9 g of KMnO4 and 2.0 mL of HCl (37 wt%) were added to 40 mL of deionized water under magnetic stirring to form the precursorsolution. After stirring the solution for about 20 min, it was transferred into an autoclave with a capacity of 100 mL. The autoclave was sealed and heated in an oven at 110 C for 24 hrs . The productwas filtered, washed with distilled water and ethanol, dried at 80 C. Preparationof Fe3O4/OMS-2 Nanotubes To fabricate the magnetic manganese oxide nanotubes, nanoparticles of Fe3O4 were deposited onto OMS-2 nanotubes using a chemical co-precipitation method [13]. 0.1 M urea extract was added to an equimolar solution of ferric chloride (FeCl3) . The resulting solution was left for stirring for 2 hours at 85-90C . 0.1 M solution of ferrous sulphate heptahydrate (FeSo4.7H2O)was added to the solution with continuous stirring for 10-15 minutes. For the formation of magnetic Fe3O4 pH of the solution was increased to maximum by addition of 0.3 M NaOH solution with continuous stirring. After 20 minutes of continuous stirring , 0.5g of the OMS-2 precursor(powder) was added to the solution. The final solution so obtained was sonicated for 15 minutes. The solution was then left for overnight aging. The productwas then washed several times with distilled water till pH became neutral ( before being separated using a magnet for magnetic separation test ). The product was then dried in an oven at 80C for 1 hour in a petridish. The dried productwas scraped of with the help of a spatula , ground into a fine powder using a pestle and mortar and stored in a cellophane pouch. Adsorption Property Measurement The reaction was carried out in 3 boiling tubes , which contained varying concentrations of lead acetate solution (0.1 M ,0.01 M ,0.05 M) prepared by dissolving appropriate quantity of lead acetated powder(analytical reagent) in distilled water, and 100 mg of composite. The mixture was allowed to react at
  10. 10. 10 room temperature with continuous stirring. The solutions were kept on stirring for about 20 minutes and then left undisturbed . After about 30-60 minutes of keeping the boiling tubes undisturbed , it was observed that that the compositecompletely adsorbs lead acetate , settles down at the bottom of each tube leaving clear water above . Sample Characterization The changes of absorptions at 221 nm were applied to identify the concentrations of lead acetate in each tube , using a LabindiaT60 UV/VIS Spectrophotometer . Plot showing concentration vs absorbance at 221nm UVradiation UV-Visible spectroscopyis used to study the interaction of the Fe3O4/OMS-2 with the lead ions. Absorptionspectra recorded in the region of 200-300 nm for 0.1 M and 0.05 M lead acetate and composite-lead acetate solution are shown in above Figure. The absorptionspectrum of lead acetate90.1 M, 0.05 M) shows the characteristic peaks at 221 nm. The spectraof lead adsorbed in both cases ( original
  11. 11. 11 lead acetate solution and clear water obtained after composite-lead acetate reaction) show difference absortion peaks signifying significant reduction of lead ions from the solution leaving clear water Result and Discussion It takes about 30 mins for all suspended particulates in the aqueous phase to be attracted and accumulated at the magnetic region (Fig. 4), indicating that the as-prepared Fe3O4/OMS-2 nanotubes exhibited remarkable magnetic separability. The sorptive degradation of heavy metals for clear water is one important wastewater treatment method nowadays. Herein, the as-prepared Fe3O4/OMS-2 nanotubes were tested for their adsorptive efficiency in the adsorption of lead acetate under controlled conditions (Fig. ). The prepared Fe3O4/OMS-2 nanotubes showed complete stability during the reaction, and 98.45 % and 99.91%(0.1 M and 0.05 M respectively) of the lead acetate was decomposed. lead acetate in 3 varying concentrations (0.1 M, 0.01 M, 0.05 M) Solutions after addition of Fe3O4-MnO2 nanotube composite (image after sedimentation ofcomposite and lead acetate
  12. 12. 12 Samples after magnetic separation ofsediment(composite-lead acetate mixtures) Future work Due to unavailability of X-Ray diffractometer , SEM and due to shortage of time - the characterization( XRD, SEM , DLS) of the Fe3O4-MnO2 nanotube composite and UV analysis of clear water obtained after reaction between the Fe3O4-MnO2 nanotube composite and 0.01 M lead acetate solution was not completed . I plan to follow up on these tasks in the current semester or in the semester break before next semester whenever time permits . Conclusion In conclusion, Fe3O4-MnO2 nanotube composite was successfully prepared by grafting Fe3O4 nanoparticles onto the OMS-2 MnO2 nanotubes. The nanotube compositeshowed excellent adsorption activity for the degradation of lead based compounds from water samples , showed 98.45% and 99.91% reduction in the concentration of lead ions from solution . The residues left at the bottom of the boiling tubes were then magnetically separated from the solution with ease leaving clear water behind . Because of its simple manipulation, the prepared composite may have potential applications in water purification technology.
  13. 13. 13 References 1. Synthesis and Catalytic Activity of Magnetic Cryptomelane-Type Manganese Oxide Nanotubes Hao-Jie Cui Jian-Wen Shi Ming-Lai Fu 2. S. L. Suib (2008). Acc. Chem. Res. 41, 479. 3. X. Wang and Y. Li (2002). J. Am. Chem. Soc. 124, 2880. 4. X. F. Shen, Y. S. Ding, J. Liu, J. Cai, K. Laubernds, R. P. Zerger, A. Vasiliev, M. Aindow, and 5. S. L. Suib (2005). Adv. Mater. 17, 805. 6. J. Luo, H. T. Zhu, H. M. Fan, J. K. Liang, H. L. Shi, G. H. Rao, J. B. Li, Z. M. Du, and Z. X. Shen 7. (2008). J. Phys. Chem. C 112, 12594. 8. H. Huang, C. H. Chen, L. Xu, H. Genuino, J. Garcia-Martinez, H. F. Garces, L. Jin, C. K. O. 9. Kithongo, and S. L. Suib (2010). Chem. Commun. 46, 5945. 10. H. J. Cui, X. H. Feng, W. F. Tan, W. Zhao, M. K. Wang, T. M. Tsao, and F. Liu (2010). Cryst. 11. Growth Des. 10, 3355. 12. M. Zhou, X. Zhang, J. Wei, S. Zhao, L. Wang, and B. Feng (2011). J. Phys. Chem. C 115, 1398. 13. H.-J. Cui, J.-W. Shi, F. Liu, and M.-L. Fu (2011). J. Mater. Chem. 21, 18527. 14. H.-J. Cui, H.-Z. Huang, M.-L. Fu, B.-L. Yuan, and W. Pearl (2011). Catal. Commun. 12, 1339. 15. B. Li, G. Rong, Y. Xie, L. Huang, and C. Feng (2006). Inorg. Chem. 45, 6404. 16. S. Chen, J. Zhu, Q. Han, Z. Zheng, Y. Yang, and X. Wang (2009). Cryst. Growth Des. 9, 4356.
  14. 14. 14 17. T. Zhang, X. Zhang, J. Ng, H. Yang, J. Liu, and D. D. Sun (2011). Chem. Commun. 47, 1890. 18. L. Li and D. L. King (2005). Chem. Mater. 17, 4335. 19. J. Chen, X. Tang, J. Liu, E. Zhan, J. Li, X. Huang, and W. Shen (2007). Chem. Mater. 19, 4292. 20. S. T. Sriskandakumar, N. Opembe, C. H. Chen, A. Morey, C. Kingondu, and S. L. Suib (2009). 21. J. Phys. Chem. A 113, 1523. 22. W. Xiao, D. Wang, and X. W. Lou (2010). J. Phys. Chem. C 114, 1694. 23. C. Burda, X. Chen, R. Narayanan, and M. A. EI-Sayed (2005). Chem. Rev. 105, 1025. 24. C. Wu and Y. Xie (2009). Chem. Commun. 40, 5943. 25. R. Wang and J. Li (2010). Environ. Sci. Technol. 11, 4282. 26. J. H. Pan, X. W. Zhang, A. J. Du, D. D. Sun, and J. O. Leckie (2008). J. Am. Chem. Soc. 130, 11256.


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