UNIVERSITY OF PETROLEUM amp ENERGY STUDIES

Dehradun

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

MINOR PROJECT

BTech MSNT(2012-16)5th - SEM

Submitted By Guided ByAnish Verma (007) GGopalakrishnanShah Faisal (42)Vishal Jain (52)Mohammad Abubakar (59)

Chapter outline of the Project

Introduction

Problem Statement

Objective

Flowchart

Methodology

MCM-41

Procedure

Synthesis

Conclusion

References

IntroductionBackground

Carbon nanotubes (CNTs) are allotropes of carbon with

a cylindrical nanostructure Nanotubes have been constructed with

length-to-diameter ratio of up to 1320000001Current applications

include Tips for atomic force microscope probes In tissue engineering

carbon nanotubes can act as scaffolding for bone growth

CNT and hetro atom substituted CNT having potential application for

Hydrogen storage devices Search for efficient H-Storage devices is

necessitated by the risk involved in transportation of hydrogen which is

regarded as potential future auto fuels

Hence efficient method of CNT amp hetro atom substituted CNT is being

sought One of the method for CNT synthesis is by catalytic CVD

(Chemical vapour deposition) and so effective efficient catalyst become

important area for research Hence it is proposed to synthesis Fe-Co

substituted MCM-41 amp characterized them for its application amp catalyst for

CNT synthesis by CVD

Problem statement

The serious problems that are affecting the development of hydrogen

cars are hydrogen storage the high reactivity of hydrogen the cost

and methods of hydrogen fuel production consumer demand and the

cost of changing the infrastructure to accommodate hydrogen

vehicles

The concerns surrounding the storage of hydrogen are a major issue

Hydrogen must be stored at extremely low temperatures and high

pressure A container capable of withstanding these specifications is

larger than a standard gas tank Hydrogen storage could be viewed

as a problem by consumers Hydrogen is extremely reactive

Hydrogen is combustible and flammable

So in order to solve the above stated problem we are making Fe-Co

substituted MCM-41 catalyst to synthesis CNT hetro atoms

substituted CNT which have the potential to be used for hydrogen

storage

Objectives

bull Develop high-capacity hydrogen storage material to meet

the demand for a hydrogen Storage system

bull To enhance the preparation of CNTrsquos produced by

Catalytic CVD using the MCM-41 Catalyst

bull Hydrogen capacity greater than 6 wt

bull Favourable thermodynamic and kinetics suitable for

transportation applications

bull Stable with hydratingdehydrating cycling

FLOWCHART OF THE PROJECT

Catalyst Analysis

Characterization and Verification of properites

Time-3-4 months

Catalyst Synthesis

Chemical preperation and synthesis

Time-4-5 months

Literature Gathering

Data collection and reading Time-3 months

Methodology

MCM-41

Mobil Composition of Matter (MCM) is the initial name given for a

series of mesoporous materials that were first synthesized by Mobils

researchers in 1992 MCM-41 (Mobil Composition of Matter No 41)

and MCM-48 (Mobil Composition of Matter No 48) are two of the most

popular mesoporous molecular sieves that are keenly studied by

researchers

The most striking fact about the MCM-41 and MCM-48 is that

although composed of amorphous silica wall they possess long range

ordered framework with uniform mesopores These materials also

possess large surface area which can be up to more than 1000 m2gminus1

Moreover the pore diameter of these materials can be nicely

controlled within mesoporous range between 15 to 20 nm by adjusting

the synthesis conditions andor by employing surfactants with different

chain lengths in their preparation

HYDROTHERMAL SYNTHESIS

bullHydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures also termed hydrothermal method

bullHydrothermal synthesis can be defined as a method of synthesis of single crystals that depends on the solubility of minerals in hot water under high pressure

PROCEDURE

Synthesis of Fe-MCM-41

Materials Required

Fe-MCM-41 molecular sieve is to be synthesised

hydrothermally using a gel composition of ndash

1SiO2001 Fe2O302 CTAB 089 H2SO4

Sodium metasilicate ferric nitrate and cetyl trimethyl

ammonium bromide(CTAB) are to be used as the sources

of silicon iron and structure-directing agent respectively

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

Chapter outline of the Project

Introduction

Problem Statement

Objective

Flowchart

Methodology

MCM-41

Procedure

Synthesis

Conclusion

References

IntroductionBackground

Carbon nanotubes (CNTs) are allotropes of carbon with

a cylindrical nanostructure Nanotubes have been constructed with

length-to-diameter ratio of up to 1320000001Current applications

include Tips for atomic force microscope probes In tissue engineering

carbon nanotubes can act as scaffolding for bone growth

CNT and hetro atom substituted CNT having potential application for

Hydrogen storage devices Search for efficient H-Storage devices is

necessitated by the risk involved in transportation of hydrogen which is

regarded as potential future auto fuels

Hence efficient method of CNT amp hetro atom substituted CNT is being

sought One of the method for CNT synthesis is by catalytic CVD

(Chemical vapour deposition) and so effective efficient catalyst become

important area for research Hence it is proposed to synthesis Fe-Co

substituted MCM-41 amp characterized them for its application amp catalyst for

CNT synthesis by CVD

Problem statement

The serious problems that are affecting the development of hydrogen

cars are hydrogen storage the high reactivity of hydrogen the cost

and methods of hydrogen fuel production consumer demand and the

cost of changing the infrastructure to accommodate hydrogen

vehicles

The concerns surrounding the storage of hydrogen are a major issue

Hydrogen must be stored at extremely low temperatures and high

pressure A container capable of withstanding these specifications is

larger than a standard gas tank Hydrogen storage could be viewed

as a problem by consumers Hydrogen is extremely reactive

Hydrogen is combustible and flammable

So in order to solve the above stated problem we are making Fe-Co

substituted MCM-41 catalyst to synthesis CNT hetro atoms

substituted CNT which have the potential to be used for hydrogen

storage

Objectives

bull Develop high-capacity hydrogen storage material to meet

the demand for a hydrogen Storage system

bull To enhance the preparation of CNTrsquos produced by

Catalytic CVD using the MCM-41 Catalyst

bull Hydrogen capacity greater than 6 wt

bull Favourable thermodynamic and kinetics suitable for

transportation applications

bull Stable with hydratingdehydrating cycling

FLOWCHART OF THE PROJECT

Catalyst Analysis

Characterization and Verification of properites

Time-3-4 months

Catalyst Synthesis

Chemical preperation and synthesis

Time-4-5 months

Literature Gathering

Data collection and reading Time-3 months

Methodology

MCM-41

Mobil Composition of Matter (MCM) is the initial name given for a

series of mesoporous materials that were first synthesized by Mobils

researchers in 1992 MCM-41 (Mobil Composition of Matter No 41)

and MCM-48 (Mobil Composition of Matter No 48) are two of the most

popular mesoporous molecular sieves that are keenly studied by

researchers

The most striking fact about the MCM-41 and MCM-48 is that

although composed of amorphous silica wall they possess long range

ordered framework with uniform mesopores These materials also

possess large surface area which can be up to more than 1000 m2gminus1

Moreover the pore diameter of these materials can be nicely

controlled within mesoporous range between 15 to 20 nm by adjusting

the synthesis conditions andor by employing surfactants with different

chain lengths in their preparation

HYDROTHERMAL SYNTHESIS

bullHydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures also termed hydrothermal method

bullHydrothermal synthesis can be defined as a method of synthesis of single crystals that depends on the solubility of minerals in hot water under high pressure

PROCEDURE

Synthesis of Fe-MCM-41

Materials Required

Fe-MCM-41 molecular sieve is to be synthesised

hydrothermally using a gel composition of ndash

1SiO2001 Fe2O302 CTAB 089 H2SO4

Sodium metasilicate ferric nitrate and cetyl trimethyl

ammonium bromide(CTAB) are to be used as the sources

of silicon iron and structure-directing agent respectively

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

IntroductionBackground

Carbon nanotubes (CNTs) are allotropes of carbon with

a cylindrical nanostructure Nanotubes have been constructed with

length-to-diameter ratio of up to 1320000001Current applications

include Tips for atomic force microscope probes In tissue engineering

carbon nanotubes can act as scaffolding for bone growth

CNT and hetro atom substituted CNT having potential application for

Hydrogen storage devices Search for efficient H-Storage devices is

necessitated by the risk involved in transportation of hydrogen which is

regarded as potential future auto fuels

Hence efficient method of CNT amp hetro atom substituted CNT is being

sought One of the method for CNT synthesis is by catalytic CVD

(Chemical vapour deposition) and so effective efficient catalyst become

important area for research Hence it is proposed to synthesis Fe-Co

substituted MCM-41 amp characterized them for its application amp catalyst for

CNT synthesis by CVD

Problem statement

The serious problems that are affecting the development of hydrogen

cars are hydrogen storage the high reactivity of hydrogen the cost

and methods of hydrogen fuel production consumer demand and the

cost of changing the infrastructure to accommodate hydrogen

vehicles

The concerns surrounding the storage of hydrogen are a major issue

Hydrogen must be stored at extremely low temperatures and high

pressure A container capable of withstanding these specifications is

larger than a standard gas tank Hydrogen storage could be viewed

as a problem by consumers Hydrogen is extremely reactive

Hydrogen is combustible and flammable

So in order to solve the above stated problem we are making Fe-Co

substituted MCM-41 catalyst to synthesis CNT hetro atoms

substituted CNT which have the potential to be used for hydrogen

storage

Objectives

bull Develop high-capacity hydrogen storage material to meet

the demand for a hydrogen Storage system

bull To enhance the preparation of CNTrsquos produced by

Catalytic CVD using the MCM-41 Catalyst

bull Hydrogen capacity greater than 6 wt

bull Favourable thermodynamic and kinetics suitable for

transportation applications

bull Stable with hydratingdehydrating cycling

FLOWCHART OF THE PROJECT

Catalyst Analysis

Characterization and Verification of properites

Time-3-4 months

Catalyst Synthesis

Chemical preperation and synthesis

Time-4-5 months

Literature Gathering

Data collection and reading Time-3 months

Methodology

MCM-41

Mobil Composition of Matter (MCM) is the initial name given for a

series of mesoporous materials that were first synthesized by Mobils

researchers in 1992 MCM-41 (Mobil Composition of Matter No 41)

and MCM-48 (Mobil Composition of Matter No 48) are two of the most

popular mesoporous molecular sieves that are keenly studied by

researchers

The most striking fact about the MCM-41 and MCM-48 is that

although composed of amorphous silica wall they possess long range

ordered framework with uniform mesopores These materials also

possess large surface area which can be up to more than 1000 m2gminus1

Moreover the pore diameter of these materials can be nicely

controlled within mesoporous range between 15 to 20 nm by adjusting

the synthesis conditions andor by employing surfactants with different

chain lengths in their preparation

HYDROTHERMAL SYNTHESIS

bullHydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures also termed hydrothermal method

bullHydrothermal synthesis can be defined as a method of synthesis of single crystals that depends on the solubility of minerals in hot water under high pressure

PROCEDURE

Synthesis of Fe-MCM-41

Materials Required

Fe-MCM-41 molecular sieve is to be synthesised

hydrothermally using a gel composition of ndash

1SiO2001 Fe2O302 CTAB 089 H2SO4

Sodium metasilicate ferric nitrate and cetyl trimethyl

ammonium bromide(CTAB) are to be used as the sources

of silicon iron and structure-directing agent respectively

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

Problem statement

The serious problems that are affecting the development of hydrogen

cars are hydrogen storage the high reactivity of hydrogen the cost

and methods of hydrogen fuel production consumer demand and the

cost of changing the infrastructure to accommodate hydrogen

vehicles

The concerns surrounding the storage of hydrogen are a major issue

Hydrogen must be stored at extremely low temperatures and high

pressure A container capable of withstanding these specifications is

larger than a standard gas tank Hydrogen storage could be viewed

as a problem by consumers Hydrogen is extremely reactive

Hydrogen is combustible and flammable

So in order to solve the above stated problem we are making Fe-Co

substituted MCM-41 catalyst to synthesis CNT hetro atoms

substituted CNT which have the potential to be used for hydrogen

storage

Objectives

bull Develop high-capacity hydrogen storage material to meet

the demand for a hydrogen Storage system

bull To enhance the preparation of CNTrsquos produced by

Catalytic CVD using the MCM-41 Catalyst

bull Hydrogen capacity greater than 6 wt

bull Favourable thermodynamic and kinetics suitable for

transportation applications

bull Stable with hydratingdehydrating cycling

FLOWCHART OF THE PROJECT

Catalyst Analysis

Characterization and Verification of properites

Time-3-4 months

Catalyst Synthesis

Chemical preperation and synthesis

Time-4-5 months

Literature Gathering

Data collection and reading Time-3 months

Methodology

MCM-41

Mobil Composition of Matter (MCM) is the initial name given for a

series of mesoporous materials that were first synthesized by Mobils

researchers in 1992 MCM-41 (Mobil Composition of Matter No 41)

and MCM-48 (Mobil Composition of Matter No 48) are two of the most

popular mesoporous molecular sieves that are keenly studied by

researchers

The most striking fact about the MCM-41 and MCM-48 is that

although composed of amorphous silica wall they possess long range

ordered framework with uniform mesopores These materials also

possess large surface area which can be up to more than 1000 m2gminus1

Moreover the pore diameter of these materials can be nicely

controlled within mesoporous range between 15 to 20 nm by adjusting

the synthesis conditions andor by employing surfactants with different

chain lengths in their preparation

HYDROTHERMAL SYNTHESIS

bullHydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures also termed hydrothermal method

bullHydrothermal synthesis can be defined as a method of synthesis of single crystals that depends on the solubility of minerals in hot water under high pressure

PROCEDURE

Synthesis of Fe-MCM-41

Materials Required

Fe-MCM-41 molecular sieve is to be synthesised

hydrothermally using a gel composition of ndash

1SiO2001 Fe2O302 CTAB 089 H2SO4

Sodium metasilicate ferric nitrate and cetyl trimethyl

ammonium bromide(CTAB) are to be used as the sources

of silicon iron and structure-directing agent respectively

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

Objectives

bull Develop high-capacity hydrogen storage material to meet

the demand for a hydrogen Storage system

bull To enhance the preparation of CNTrsquos produced by

Catalytic CVD using the MCM-41 Catalyst

bull Hydrogen capacity greater than 6 wt

bull Favourable thermodynamic and kinetics suitable for

transportation applications

bull Stable with hydratingdehydrating cycling

FLOWCHART OF THE PROJECT

Catalyst Analysis

Characterization and Verification of properites

Time-3-4 months

Catalyst Synthesis

Chemical preperation and synthesis

Time-4-5 months

Literature Gathering

Data collection and reading Time-3 months

Methodology

MCM-41

Mobil Composition of Matter (MCM) is the initial name given for a

series of mesoporous materials that were first synthesized by Mobils

researchers in 1992 MCM-41 (Mobil Composition of Matter No 41)

and MCM-48 (Mobil Composition of Matter No 48) are two of the most

popular mesoporous molecular sieves that are keenly studied by

researchers

The most striking fact about the MCM-41 and MCM-48 is that

although composed of amorphous silica wall they possess long range

ordered framework with uniform mesopores These materials also

possess large surface area which can be up to more than 1000 m2gminus1

Moreover the pore diameter of these materials can be nicely

controlled within mesoporous range between 15 to 20 nm by adjusting

the synthesis conditions andor by employing surfactants with different

chain lengths in their preparation

HYDROTHERMAL SYNTHESIS

bullHydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures also termed hydrothermal method

bullHydrothermal synthesis can be defined as a method of synthesis of single crystals that depends on the solubility of minerals in hot water under high pressure

PROCEDURE

Synthesis of Fe-MCM-41

Materials Required

Fe-MCM-41 molecular sieve is to be synthesised

hydrothermally using a gel composition of ndash

1SiO2001 Fe2O302 CTAB 089 H2SO4

Sodium metasilicate ferric nitrate and cetyl trimethyl

ammonium bromide(CTAB) are to be used as the sources

of silicon iron and structure-directing agent respectively

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

FLOWCHART OF THE PROJECT

Catalyst Analysis

Characterization and Verification of properites

Time-3-4 months

Catalyst Synthesis

Chemical preperation and synthesis

Time-4-5 months

Literature Gathering

Data collection and reading Time-3 months

Methodology

MCM-41

Mobil Composition of Matter (MCM) is the initial name given for a

series of mesoporous materials that were first synthesized by Mobils

researchers in 1992 MCM-41 (Mobil Composition of Matter No 41)

and MCM-48 (Mobil Composition of Matter No 48) are two of the most

popular mesoporous molecular sieves that are keenly studied by

researchers

The most striking fact about the MCM-41 and MCM-48 is that

although composed of amorphous silica wall they possess long range

ordered framework with uniform mesopores These materials also

possess large surface area which can be up to more than 1000 m2gminus1

Moreover the pore diameter of these materials can be nicely

controlled within mesoporous range between 15 to 20 nm by adjusting

the synthesis conditions andor by employing surfactants with different

chain lengths in their preparation

HYDROTHERMAL SYNTHESIS

bullHydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures also termed hydrothermal method

bullHydrothermal synthesis can be defined as a method of synthesis of single crystals that depends on the solubility of minerals in hot water under high pressure

PROCEDURE

Synthesis of Fe-MCM-41

Materials Required

Fe-MCM-41 molecular sieve is to be synthesised

hydrothermally using a gel composition of ndash

1SiO2001 Fe2O302 CTAB 089 H2SO4

Sodium metasilicate ferric nitrate and cetyl trimethyl

ammonium bromide(CTAB) are to be used as the sources

of silicon iron and structure-directing agent respectively

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

Methodology

MCM-41

Mobil Composition of Matter (MCM) is the initial name given for a

series of mesoporous materials that were first synthesized by Mobils

researchers in 1992 MCM-41 (Mobil Composition of Matter No 41)

and MCM-48 (Mobil Composition of Matter No 48) are two of the most

popular mesoporous molecular sieves that are keenly studied by

researchers

The most striking fact about the MCM-41 and MCM-48 is that

although composed of amorphous silica wall they possess long range

ordered framework with uniform mesopores These materials also

possess large surface area which can be up to more than 1000 m2gminus1

Moreover the pore diameter of these materials can be nicely

controlled within mesoporous range between 15 to 20 nm by adjusting

the synthesis conditions andor by employing surfactants with different

chain lengths in their preparation

HYDROTHERMAL SYNTHESIS

bullHydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures also termed hydrothermal method

bullHydrothermal synthesis can be defined as a method of synthesis of single crystals that depends on the solubility of minerals in hot water under high pressure

PROCEDURE

Synthesis of Fe-MCM-41

Materials Required

Fe-MCM-41 molecular sieve is to be synthesised

hydrothermally using a gel composition of ndash

1SiO2001 Fe2O302 CTAB 089 H2SO4

Sodium metasilicate ferric nitrate and cetyl trimethyl

ammonium bromide(CTAB) are to be used as the sources

of silicon iron and structure-directing agent respectively

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

HYDROTHERMAL SYNTHESIS

bullHydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures also termed hydrothermal method

bullHydrothermal synthesis can be defined as a method of synthesis of single crystals that depends on the solubility of minerals in hot water under high pressure

PROCEDURE

Synthesis of Fe-MCM-41

Materials Required

Fe-MCM-41 molecular sieve is to be synthesised

hydrothermally using a gel composition of ndash

1SiO2001 Fe2O302 CTAB 089 H2SO4

Sodium metasilicate ferric nitrate and cetyl trimethyl

ammonium bromide(CTAB) are to be used as the sources

of silicon iron and structure-directing agent respectively

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

PROCEDURE

Synthesis of Fe-MCM-41

Materials Required

Fe-MCM-41 molecular sieve is to be synthesised

hydrothermally using a gel composition of ndash

1SiO2001 Fe2O302 CTAB 089 H2SO4

Sodium metasilicate ferric nitrate and cetyl trimethyl

ammonium bromide(CTAB) are to be used as the sources

of silicon iron and structure-directing agent respectively

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

Synthesis of catalyst

In a typical synthesis 212g of sodium metasilicate is added with ferric

nitrate and dissolved in distilled water The pH of the solution is adjusted to

105 using 1M sulphuric acid and the content was stirred well to form a gel

An aqueous solution of CTAB was prepared by dissolving 72 g of it in

distilled water and it is added slowly to the gel for a period of about 30 min

The resulting mixture is then stirred for 1 hrs at room temperature and

autoclaved at 145oC for 48 hr The crystallized Fe-MCM-41 is recovered by

filtration washed several times with distilled water and dried at 80oC for 3

HrThe occluded surfactant was removed by calcination at 550oC in muffle

furnace for 6 hrs to obtain Fe-MCM-41

Synthesis of Fe-MCM-41 and Co-MCM-41

Co-MCM-41 is synthesised by adopting the above procedure in which

cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe

(ratio 11)

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

CONCLUSION

The synthesis of the Fe-Co-MCM-41

catalyst for the catalytic CVD synthesis

of CNTrsquos will be carried out

successfully

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193

REFERENCES

1 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

2 Laudise RA (1958) RH Doremus BW 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 27ndash29 1958 Wiley New York pp 458ndash

463

3 Chronological reference marks - Charles Chamberland (1851ndash1908) Pasteur

InstituteArchived from the original on 19 December 2006 Retrieved 2007-01-19

4 Hugo WB (July 1991) A brief history of heat and chemical preservation and

disinfectionJ Appl Bacteriol 71 (1) 9ndash18 doi101111j1365-

26721991tb04657x PMID 1894581

5 Bulletin - United States Geological Survey Issues 47-54 1889 pp 180 (834)

6 Electric Muffle Furnace CA Crowley Popular Mechanics 676 June 1937 pp 941-

945

7 JS Beck et alJ Am Chem Soc 114 (1992) 10834

8 T Somanathan A Pandurangan et al AChem256 (2006) 193