Minor ppt EndSem

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22-11-2014

B.Tech MSNT 5Th SEM

MINOR PROJECT PRESENTATION

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UNIVERSITY OF PETROLEUM & ENERGY STUDIES Dehradun

The Synthesis of Fe-Co MCM-41 Catalyst for the preparation of Carbon nanotubes by Catalytic Chemical Vapor Deposition

MINOR PROJECT

B.Tech MSNT(2012-16)5th - SEM

Submitted By: Guided By:Anish Verma (007) Dr. G.GopalakrishnanShah Faisal (42)Vishal Jain (52)Mohammad Abubakar (59)

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PROBLEM STATEMENT

The serious problems to use hydrogen as a fuel is hydrogen storage and transportation due to the high reactivity of hydrogen ,so to stored

this we are making CNT’s by using of MCM-41 catalyst .To use hydrogen as a future fuel.

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INTRODUCTION

Potentially, Hydrogen can be used as a fuel and can act as a substitute for petroleum-based fuels in later stages. The major reason for it is:

•Environmental friendly as the resultant product we obtain is water only by Combustion of H fuel.

But unfortunately Hydrogen fuel is not being commercially used as the storage of Hydrogen is a big concern due to requirement of cryogenic environment and highly insulated storage tanks.

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WHAT IS MCM 41 ?

•Mobil Composition of Matter No. 41•Mesoporous material with a hierarchical structure from a family of silicates.•Used as catalysts for various chemical reactions, as a support for drug delivery system and as adsorbent in waste water treatment.

MCM-41 Synthesis

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MCM-41

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OBJECTIVE

To achieve high purity and high performance of the catalyst.

•Synthesis of Fe-Co MCM-41 Catalyst with varying the molar ratios of Fe,Co with respect to Si.

•Characterization of synthesized catalyst by XRD, FT-IR.

•Optimization of catalyst conditions (purity and structure) after analysing its properties

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Measure the average spacing between layers or rows of atoms.

Determine the orientation of a single crystal or grain.

Find the crystal structure of an unknown material. Measure the size, shape and internal stress of small crystalline regions.

Why XRD?

Bruker D8 Advance Diffractometer

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It can identify unknown materials

metal bandsIt can determine the quality or consistency

of a sampleComposition of the material such as Metal

oxides

WHY FT-IR ?

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SYNTHESIS OF Fe MCM-41 Sodium metasilicate+50ml H2O

( 30 min stirring) Fe(NO3)3.9H2O+10ml H2O

1hr stirring2N H2SO4(80ml)

2hr stirringCTAB+ 20ml H2O

2hr stirringTransfer to Autoclave and keep in oven 145-1500C for 48 hours

Remove from hot air oven ( 2-3 hr cooling) Remove from autoclave

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SYNTHESIS OF Fe MCM-41 Filtration with Deionized water

( pH<10) Drying in oven

4hr 80-1000C Remove and allow to cool

1-2hr Calcination

5500C for 6 hoursRemove and allow to cool

Fe-MCM-41

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Co MCM-41 Fe-Co MCM-41 Fe MCM-41

Samples Prepared:

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STANDARD PEAKS

Characterization

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Fe XRD RESULT(Sample not formed)

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FT-IR RESULT(Fe-Co)

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 •A broad band around 3442.92 cm-1 is due to OH stretching of water. The broad band between 1300 and 1000 cm-1 (1098.89 cm-1) is due to internal and external asymmetric Si-O-Si stretching modes. The band at 805.07 cm-1 is assigned to symmetric stretching of Si-O-Si.

FTIR ANALYSIS

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From the low angle XRD pattern on comparing with the standard result the peak came between 2 & 3 degree but the peak was very low intensity for Fe MCM-41 which suggest that catalyst was not formed.From high angle XRD pattern another peak was found which correspond to Fe2O3.

From FT-IR before and after calcination the changes in peak which suggest that calcination is complete.We also found that improper mixing of the gel formed, led us to the deviation from MCM-41 Structure.

Result and Analysis

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• Synthesize Fe-Co of different ratios with respect to Si by varying other parameters such as crystallization time.

• To recheck the procedure steps involved to improve the yield and prevent impurities.

• To synthesize MCM-41 catalyst for CNT preparation.

• Analyze the results for changes and evaluate for proficiency.

Future Working

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•  Reichinger, M., Poröse Silikate mit hierarchischer Porenstruktur: Synthese von mikro-/mesoporösem MCM-41 und MCM-48 Materialien aus zeolithischen Baueinheiten des MFI-Gerüststrukturtyps, Dissertation Ruhr-Universität Bochum, 2007

• Silaghi, M.-C., Chizallet, C., Raybaud, P.; Challenges on molecular aspects of dealumination and desilication of zeolites, Microporous and Mesoporous Materials, 191 (2014) 82-96.

• Laudise, R.A. (1958). R.H. Doremus, B.W. Roberts and D. Turnbull, ed. Growth and perfection of crystals. Proceedings of an International Conference on Crystal Growth held at Cooperstown, New York on August 27–29, 1958. Wiley, New York. pp. 458–463.

• "Chronological reference marks - Charles Chamberland (1851–1908)". Pasteur Institute.Archived from the original on 19 December 2006. Retrieved 2007-01-19.

• Hugo WB (July 1991). "A brief history of heat and chemical preservation and disinfection".J. Appl. Bacteriol. 71 (1): 9–18. doi:10.1111/j.1365-2672.1991.tb04657.x. PMID 1894581.

• Bulletin - United States Geological Survey, Issues 47-54, 1889, pp. 180 (834)• Electric Muffle Furnace, C.A. Crowley, Popular Mechanics, 67:6, June 1937, pp. 941-945• J.S. Beck, et al.,J. Am. Chem. Soc. 114 (1992) 10834.• T. Somanathan, A. Pandurangan, et. al. A:Chem.256 (2006) 193.

References