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
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