WO2023170708A1 - Sustainable reclamation of bio mass - Google Patents

Sustainable reclamation of bio mass Download PDF

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Publication number
WO2023170708A1
WO2023170708A1 PCT/IN2023/050222 IN2023050222W WO2023170708A1 WO 2023170708 A1 WO2023170708 A1 WO 2023170708A1 IN 2023050222 W IN2023050222 W IN 2023050222W WO 2023170708 A1 WO2023170708 A1 WO 2023170708A1
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bio mass
carbon nanoparticles
duration
heating
powder
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PCT/IN2023/050222
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French (fr)
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Gurumurthy Hegde
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Christ (Deemed To Be University)
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter

Definitions

  • the invention generally relates to the field of sustainable reclamation of bio mass and more particularly to a method for sustainable reclamation of bio mass for obtaining carbon nanoparticles.
  • Carbon nanoparticles and particularly hollow/porous carbon nanoparticles are a class of carbon nanostructures having a singular architecture consisting of a porous carbon shell enclosing a large internal void.
  • the hollow carbon nanoparticles have a wide range of applications including but not limited to electrochemical energy storage, heterogeneous catalysis, adsorption, water purification, carbon capture, electromagnetic shielding and biomedical applications (like biodiagnostics and drug delivery).
  • Bio mass are non-fossil resources of organic origin that are available on renewable, sustainable, clean and recurring bases.
  • Bio mass materials particularly agro-based bio mass include leaves, stalk, stem, husk, saw dust, peelings obtained from plants. Bio mass materials are seen as affordable alternative to conventional materials for domestic and industrial applications.
  • Carbon nanoparticles are obtained from a variety of sources using various fabrication methods. Graphite powders, petroleum pitch, carbon rich polymers, liquid hydrocarbons and gaseous hydrocarbons are extensively used as source for synthesizing carbon nanoparticles. The above mentioned sources being scarce and having detrimental effect on environment, there is need for an alternative carbon source.
  • the fabrication method of carbon nanoparticles is usually based on templating methodologies. Through templating technique porous carbon nanoparticles can be produced directly without the need of activation step, simply by removing the template. Depending on the nature of template used for fabrication, two types of pathways are distinguished. The hard template method is commonly based on use of silica materials as template.
  • Silica material includes but is not limited to porous silica, mesoporous silica, colloidal silica nanoparticles and zeolite.
  • the soft template method is based on use of organic molecules as templates.
  • the material used for soft template include but is not limited to surface micelles, liquid crystalline phases, surfactants, core shell particles, colloidal particles, phenolic resins and aniline oligomers.
  • One significant disadvantage of template methodology is of upscaling them for industrial purposes. As the synthesis protocols used in templating approaches generally require numerous steps, use of expensive ingredients and particularly, in case of silica based hard templating routes, use of harmful substances(ex HF and NaOH) to remove the template.
  • Fig.1 shows a thermal gravimetric analysis of the biomass arecanut, according to an example of the invention.
  • Fig.2 shows a FESEM image of the synthesized carbon nanoparticles and the corresponding nano sizes of the carbon nanoparticles at various temperatures, according to an example of the invention.
  • Fig. 3 shows a FESEM EDX spectrum of the synthesized carbon nanoparticles and their corresponding elemental analysis according to an example of the invention.
  • Fig. 4 shows a X-ray diffraction spectrum and Raman spectra of the synthesized carbon nanoparticles, according to an example of the invention.
  • Fig. 5 shows a FTIR spectrum of the precursor and the synthesized carbon nanoparticles at various temperatures, according to an example of the invention.
  • Fig. 6 shows a BET surface area of the synthesized nanoparticles at 1000°C and corresponding BET surface area values and the synthesized carbon nanoparticles at various temperatures, according to an example of the invention.
  • Fig. 7 shows a TEM image of the synthesized carbon nanoparticles and their porous nature, according to an example of the invention.
  • One aspect of the invention provides a method for sustainable reclamation of bio mass for obtaining carbon nanoparticles.
  • the method includes obtaining the bio mass in powder form, subjecting the bio mass powder to an initial rapid heating from 100 °C to 600 °C for a predetermined first duration of time for removal of organic matter to obtain a residue, initiating a second slow heating step on the obtained residue for a predetermined second duration of time to obtain an intermediate and cooling down the intermediate at a rate of 10 °C per minute to obtain spherical shaped porous carbon nanoparticles.
  • the heating and the cooling steps are performed under anaerobic conditions.
  • Various embodiments of the invention provide a method for sustainable reclamation of bio mass for obtaining carbon nanoparticles.
  • the method includes obtaining the bio mass in powder form, subjecting the bio mass powder to an initial rapid heating step at a temperature ranging from 100 °C to 600 °C for a predetermined first duration of time for removal of organic matter to obtain a residue.
  • the rapid heating is followed by initiating a second slow heating step on the obtained residue for a predetermined second duration of time to obtain an intermediate.
  • the residue is heated upto a temperature of 600 °C to 1000 °C for a time duration of 40 minutes to 45 minutes.
  • the slow heating is achieved by heating the residue gradually at a rate of 5 °C per minute till a desired temperature ranging from 600 °C to 1000 °C is reached to obtain the intermediate.
  • the temperature conditions are maintained for 60 minutes to stabilize the system.
  • the heating step is followed by cooling the intermediate at a rate of 10 °C per minute to obtain carbon nanoparticles.
  • the method for sustainable reclamation of bio mass for obtaining carbon nanoparticles includes obtaining the bio mass in powder form.
  • the bio mass includes plant based bio mass, the plant based bio mass includes but is not limited to agricultural waste, fruit peels, vegetable peels, fruit seeds, palm leaves, palm nut, arecanut and plant leaves.
  • the bio mass is obtained in powder form by heating the bio mass at a temperature ranging from 80 °C to 100 °C to remove moisture followed by grinding and sieving to obtain bio mass powder with grain size ranging from 50 to 100 urn.
  • the bio mass powder is subjected to an initial rapid heating step at a temperature ranging from 100 °C to 600 °C for a predetermined first duration of time for removal of organic matter to obtain a residue.
  • the predetermined first duration of time ranges from 20 minutes to 70 minutes. Rapid heating of the bio mass at the elevated temperature results in removal of the organic matter.
  • the heating of the bio mass powder is carried out in a tube furnace under controlled temperature and anaerobic conditions.
  • the anaerobic condition is maintained by continuous flow of an inert gas at rate of 100 ml /cm 3 -150 ml /cm 3 .
  • the anaerobic condition is maintained by continuous flow of nitrogen gas at rate of 100-150 ml /cm 3 .
  • the residue obtained after first heating step is subjected to a second slow heating step for a predetermined second duration of time to obtain an intermediate.
  • the residue is heated upto a temperature of 600 °C to 1000 °C for a time duration of 40 minutes to 45 minutes.
  • the slow heating is achieved by heating the residue gradually by increasing the temperature at a rate of 5 °C per minute till a desired temperature ranging from 600 °C to 1000 °C is reached to obtain the intermediate.
  • the temperature conditions are maintained for 60 minutes to stabilize the system.
  • the slow heating of the residue is carried out in a furnace under controlled temperature and anaerobic conditions.
  • the anaerobic condition is maintained by continuous flow of an inert gas at rate of 100-150 ml /cm 3 .
  • the anaerobic condition is maintained by continuous flow of nitrogen gas at rate of 100-150 ml /cm 3 .
  • the heating step is followed by cooling the intermediate at a rate of 10 °C per minute to obtain carbon nanoparticles.
  • the particle size of carbon nanoparticles ranges from 20 nm to 100 nm depending on applications.
  • the method of sustainable reclamation of bio mass for obtaining carbon nanoparticles as disclosed herein has a yield of carbon nanoparticles in the range of 97% to 99%.
  • arecanut is selected as the plant based bio mass for the sustainable reclamation to obtain carbon nanoparticles.
  • Arecanut is obtained in the powder form by heating the arecanut at a temperature ranging from 80 °C to 100 °C to remove moisture followed by grinding and sieving to obtain arecanut powder with grain size ranging from 50 to 100 urn.
  • the arecanut powder is subjected to an initial rapid heating step at a temperature ranging from 500 °C to 600 °C for a predetermined first duration of time for removal of organic matter to obtain a residue.
  • the predetermined first duration of time ranges from 20 minutes to 70 minutes.
  • Rapid heating of the arecanut powder at the elevated temperature results in removal of the organic matter.
  • the heating of the arecanut powder is carried out in a furnance under controlled temperature and anaerobic conditions.
  • the anaerobic condition is maintained by continuous flow of nitrogen gas at rate of 100-150 ml /cm 3 .
  • the residue obtained after first heating step is subjected to a second slow heating step for a predetermined second duration of time to obtain an intermediate.
  • the residue is heated upto a temperature of 600 °C to 1000 °C for a time duration of 40 minutes to 45 minutes.
  • the slow heating is achieved by heating the residue gradually by increasing the temperature at a rate of 5 °C per minute till a desired temperature ranging from 600 °C to 1000 °C is reached to obtain the intermediate.
  • the temperature conditions are maintained for 60 minutes to stabilize the system.
  • the slow heating of the residue is carried out in a tube furnance under controlled temperature and anaerobic conditions.
  • the anaerobic condition is maintained by continuous flow of nitrogen gas at rate of 100- 150 ml /cm 3 .
  • the heating step is followed by cooling the intermediate at a rate of 10 °C per minute to obtain carbon nanoparticles.
  • the particle size of carbon nanoparticles ranges from 20 nm to 100 nm.
  • the carbon nanoparticles obtained are characterized and evaluated using various analysis methods.
  • Fig. 1 shows a thermal gravimetric analysis of the biomass arecanut, according to an example of the invention. The figure reveals that after 600°C, almost all lignocellulosic material is degraded and only majority carbon remains.
  • Fig.2 shows a FESEM image of the synthesized carbon nanoparticles at 1000°C, according to an example of the invention.
  • the image shows that the shape of the carbon nanoparticles as obtained in the present invention is uniform and the size of the nanoparticles ranges from about 40nm to 100 nm.
  • Fig. 3 shows a FESEM EDX spectrum of the synthesized carbon nanoparticles, according to an example of the invention.
  • the FESEM EDX data reveal that obtained carbon nanoparticles contain about 98% carbon at various temperatures.
  • Fig. 4 shows a X-ray diffraction spectrum and Raman spectrum of the synthesized carbon nanoparticles, according to an example of the invention.
  • Fig. 5 shows a FTIR spectrum of the synthesized carbon nanoparticles at various temperatures, according to an example of the invention.
  • the FTIR spectrum shows maximum peak value to evident the presence of carbon.
  • Fig. 6 shows a BET surface area data of the synthesized carbon nanoparticles, according to an example of the invention. BET suggests that the nanoparticles obtained at 1000°C had highest surface area.
  • Fig. 7 shows a TEM image of the synthesized carbon nanoparticles, according to an example of the invention.
  • the TEM image shows that the carbon nanoparticles obtained from arecanut are spherical in shape and are porous in nature.
  • the method of sustainable reclamation of the bio mass for obtaining carbon nanoparticles advantageously provide a sustainable method for using the bio mass through the production of carbon nanoparticles that are very small in the size (20-1 OOnm) and are porous in nature making them suitable for a wide range of applications including but not limited to electrochemical energy storage, heterogeneous catalysis, adsorption, water purification, carbon capture, electromagnetic shielding and biomedical applications (like biodiagnostics and drug delivery). Further, the method yields carbon nanoparticles from bio mass in the range of 97% to 99%.

Abstract

The invention provides a method for sustainable reclamation of bio mass for obtaining porous carbon nanoparticles. The method 5 includes obtaining the bio mass in powder form and subjecting the bio mass powder to an initial rapid heating from 100oC to 600oC for a predetermined first duration of time for removal of organic matter to obtain a residue. Rapid heating is followed by a second slow heating step on the obtained residue for a 10 predetermined second duration of time to obtain an intermediate. In the second slow heating step, the residue is heated upto a temperature of 6000C to 10000C for a time duration of 40 minutes to 45 minutes and cooling down the intermediate at a rate of 10oC per minute to obtain carbon 15 nanoparticles. The heating and the cooling steps are performed under anaerobic conditions. The particle size of carbon nanoparticles ranges from 20nm to 100nm.

Description

SUSTAINABLE RECLAMATION OF BIO MASS
FIELD OF INVENTION
The invention generally relates to the field of sustainable reclamation of bio mass and more particularly to a method for sustainable reclamation of bio mass for obtaining carbon nanoparticles.
BACKGROUND
Carbon nanoparticles and particularly hollow/porous carbon nanoparticles are a class of carbon nanostructures having a singular architecture consisting of a porous carbon shell enclosing a large internal void. The hollow carbon nanoparticles have a wide range of applications including but not limited to electrochemical energy storage, heterogeneous catalysis, adsorption, water purification, carbon capture, electromagnetic shielding and biomedical applications (like biodiagnostics and drug delivery).
Bio mass are non-fossil resources of organic origin that are available on renewable, sustainable, clean and recurring bases. Bio mass materials particularly agro-based bio mass include leaves, stalk, stem, husk, saw dust, peelings obtained from plants. Bio mass materials are seen as affordable alternative to conventional materials for domestic and industrial applications.
Carbon nanoparticles are obtained from a variety of sources using various fabrication methods. Graphite powders, petroleum pitch, carbon rich polymers, liquid hydrocarbons and gaseous hydrocarbons are extensively used as source for synthesizing carbon nanoparticles. The above mentioned sources being scarce and having detrimental effect on environment, there is need for an alternative carbon source. The fabrication method of carbon nanoparticles is usually based on templating methodologies. Through templating technique porous carbon nanoparticles can be produced directly without the need of activation step, simply by removing the template. Depending on the nature of template used for fabrication, two types of pathways are distinguished. The hard template method is commonly based on use of silica materials as template. Silica material includes but is not limited to porous silica, mesoporous silica, colloidal silica nanoparticles and zeolite. The soft template method is based on use of organic molecules as templates. The material used for soft template include but is not limited to surface micelles, liquid crystalline phases, surfactants, core shell particles, colloidal particles, phenolic resins and aniline oligomers. One significant disadvantage of template methodology is of upscaling them for industrial purposes. As the synthesis protocols used in templating approaches generally require numerous steps, use of expensive ingredients and particularly, in case of silica based hard templating routes, use of harmful substances(ex HF and NaOH) to remove the template.
Hence, there is a need to look not only for alternative source of carbon that are abundantly available and can be used sustainably, but also for sustainable methods for obtaining carbon nanoparticles.
BRIEF DESCRIPTION OF DRAWINGS
So that the manner in which the recited features of the invention can be understood in detail, some of the embodiments are illustrated in the appended drawings. It is to be noted, however, that the appended drawings illustrate only typical embodiments of this invention and are therefore not to be considered limiting of its scope, for the invention may admit to other equally effective embodiments.
Fig.1 shows a thermal gravimetric analysis of the biomass arecanut, according to an example of the invention.
Fig.2 shows a FESEM image of the synthesized carbon nanoparticles and the corresponding nano sizes of the carbon nanoparticles at various temperatures, according to an example of the invention.
Fig. 3 shows a FESEM EDX spectrum of the synthesized carbon nanoparticles and their corresponding elemental analysis according to an example of the invention.
Fig. 4 shows a X-ray diffraction spectrum and Raman spectra of the synthesized carbon nanoparticles, according to an example of the invention.
Fig. 5 shows a FTIR spectrum of the precursor and the synthesized carbon nanoparticles at various temperatures, according to an example of the invention. Fig. 6 shows a BET surface area of the synthesized nanoparticles at 1000°C and corresponding BET surface area values and the synthesized carbon nanoparticles at various temperatures, according to an example of the invention.
Fig. 7 shows a TEM image of the synthesized carbon nanoparticles and their porous nature, according to an example of the invention.
SUMMARY OF THE INVENTION
One aspect of the invention provides a method for sustainable reclamation of bio mass for obtaining carbon nanoparticles. The method includes obtaining the bio mass in powder form, subjecting the bio mass powder to an initial rapid heating from 100 °C to 600 °C for a predetermined first duration of time for removal of organic matter to obtain a residue, initiating a second slow heating step on the obtained residue for a predetermined second duration of time to obtain an intermediate and cooling down the intermediate at a rate of 10 °C per minute to obtain spherical shaped porous carbon nanoparticles. The heating and the cooling steps are performed under anaerobic conditions.
DETAILED DESCRIPTION OF THE INVENTION
Various embodiments of the invention provide a method for sustainable reclamation of bio mass for obtaining carbon nanoparticles. The method includes obtaining the bio mass in powder form, subjecting the bio mass powder to an initial rapid heating step at a temperature ranging from 100 °C to 600 °C for a predetermined first duration of time for removal of organic matter to obtain a residue. The rapid heating is followed by initiating a second slow heating step on the obtained residue for a predetermined second duration of time to obtain an intermediate. In the second slow heating step, the residue is heated upto a temperature of 600 °C to 1000 °C for a time duration of 40 minutes to 45 minutes. The slow heating is achieved by heating the residue gradually at a rate of 5 °C per minute till a desired temperature ranging from 600 °C to 1000 °C is reached to obtain the intermediate. The temperature conditions are maintained for 60 minutes to stabilize the system. Then the heating step is followed by cooling the intermediate at a rate of 10 °C per minute to obtain carbon nanoparticles. The method described herein briefly shall now be explained in detail below. The method for sustainable reclamation of bio mass for obtaining carbon nanoparticles includes obtaining the bio mass in powder form. The bio mass includes plant based bio mass, the plant based bio mass includes but is not limited to agricultural waste, fruit peels, vegetable peels, fruit seeds, palm leaves, palm nut, arecanut and plant leaves.
The bio mass is obtained in powder form by heating the bio mass at a temperature ranging from 80 °C to 100 °C to remove moisture followed by grinding and sieving to obtain bio mass powder with grain size ranging from 50 to 100 urn. The bio mass powder is subjected to an initial rapid heating step at a temperature ranging from 100 °C to 600 °C for a predetermined first duration of time for removal of organic matter to obtain a residue. The predetermined first duration of time ranges from 20 minutes to 70 minutes. Rapid heating of the bio mass at the elevated temperature results in removal of the organic matter. The heating of the bio mass powder is carried out in a tube furnace under controlled temperature and anaerobic conditions. The anaerobic condition is maintained by continuous flow of an inert gas at rate of 100 ml /cm3-150 ml /cm3. In one embodiment of the invention, the anaerobic condition is maintained by continuous flow of nitrogen gas at rate of 100-150 ml /cm3. The residue obtained after first heating step is subjected to a second slow heating step for a predetermined second duration of time to obtain an intermediate. In the second slow heating step, the residue is heated upto a temperature of 600 °C to 1000 °C for a time duration of 40 minutes to 45 minutes. The slow heating is achieved by heating the residue gradually by increasing the temperature at a rate of 5 °C per minute till a desired temperature ranging from 600 °C to 1000 °C is reached to obtain the intermediate. The temperature conditions are maintained for 60 minutes to stabilize the system. The slow heating of the residue is carried out in a furnace under controlled temperature and anaerobic conditions. The anaerobic condition is maintained by continuous flow of an inert gas at rate of 100-150 ml /cm3. In one embodiment of the invention, the anaerobic condition is maintained by continuous flow of nitrogen gas at rate of 100-150 ml /cm3. The heating step is followed by cooling the intermediate at a rate of 10 °C per minute to obtain carbon nanoparticles. The particle size of carbon nanoparticles ranges from 20 nm to 100 nm depending on applications. The method of sustainable reclamation of bio mass for obtaining carbon nanoparticles as disclosed herein has a yield of carbon nanoparticles in the range of 97% to 99%.
The method of sustainable reclamation of bio mass for obtaining carbon nanoparticles as disclosed herein above shall be explained with an example. In an example of the invention, arecanut is selected as the plant based bio mass for the sustainable reclamation to obtain carbon nanoparticles. Arecanut is obtained in the powder form by heating the arecanut at a temperature ranging from 80 °C to 100 °C to remove moisture followed by grinding and sieving to obtain arecanut powder with grain size ranging from 50 to 100 urn. The arecanut powder is subjected to an initial rapid heating step at a temperature ranging from 500 °C to 600 °C for a predetermined first duration of time for removal of organic matter to obtain a residue. The predetermined first duration of time ranges from 20 minutes to 70 minutes. Rapid heating of the arecanut powder at the elevated temperature results in removal of the organic matter. The heating of the arecanut powder is carried out in a furnance under controlled temperature and anaerobic conditions. The anaerobic condition is maintained by continuous flow of nitrogen gas at rate of 100-150 ml /cm3. The residue obtained after first heating step is subjected to a second slow heating step for a predetermined second duration of time to obtain an intermediate. In the second slow heating step, the residue is heated upto a temperature of 600 °C to 1000 °C for a time duration of 40 minutes to 45 minutes. The slow heating is achieved by heating the residue gradually by increasing the temperature at a rate of 5 °C per minute till a desired temperature ranging from 600 °C to 1000 °C is reached to obtain the intermediate. The temperature conditions are maintained for 60 minutes to stabilize the system. The slow heating of the residue is carried out in a tube furnance under controlled temperature and anaerobic conditions. The anaerobic condition is maintained by continuous flow of nitrogen gas at rate of 100- 150 ml /cm3. The heating step is followed by cooling the intermediate at a rate of 10 °C per minute to obtain carbon nanoparticles. The particle size of carbon nanoparticles ranges from 20 nm to 100 nm. The carbon nanoparticles obtained are characterized and evaluated using various analysis methods.
Fig. 1 shows a thermal gravimetric analysis of the biomass arecanut, according to an example of the invention. The figure reveals that after 600°C, almost all lignocellulosic material is degraded and only majority carbon remains.
Fig.2 shows a FESEM image of the synthesized carbon nanoparticles at 1000°C, according to an example of the invention. The image shows that the shape of the carbon nanoparticles as obtained in the present invention is uniform and the size of the nanoparticles ranges from about 40nm to 100 nm. Fig. 3 shows a FESEM EDX spectrum of the synthesized carbon nanoparticles, according to an example of the invention. The FESEM EDX data reveal that obtained carbon nanoparticles contain about 98% carbon at various temperatures. Fig. 4 shows a X-ray diffraction spectrum and Raman spectrum of the synthesized carbon nanoparticles, according to an example of the invention. The X-ray diffraction spectrum shows the evidence of presence of the carbon in the product obtained after subjecting the arecanut powder to the heating steps whereas Raman shows the degeneracy present in the material. Fig. 5 shows a FTIR spectrum of the synthesized carbon nanoparticles at various temperatures, according to an example of the invention. The FTIR spectrum shows maximum peak value to evident the presence of carbon.
Fig. 6 shows a BET surface area data of the synthesized carbon nanoparticles, according to an example of the invention. BET suggests that the nanoparticles obtained at 1000°C had highest surface area.
Fig. 7 shows a TEM image of the synthesized carbon nanoparticles, according to an example of the invention. The TEM image shows that the carbon nanoparticles obtained from arecanut are spherical in shape and are porous in nature.
The method of sustainable reclamation of the bio mass for obtaining carbon nanoparticles advantageously provide a sustainable method for using the bio mass through the production of carbon nanoparticles that are very small in the size (20-1 OOnm) and are porous in nature making them suitable for a wide range of applications including but not limited to electrochemical energy storage, heterogeneous catalysis, adsorption, water purification, carbon capture, electromagnetic shielding and biomedical applications (like biodiagnostics and drug delivery). Further, the method yields carbon nanoparticles from bio mass in the range of 97% to 99%.
The foregoing description of the invention has been set merely to illustrate the invention and is not intended to be limiting. Since modifications of the disclosed embodiments incorporating the spirit and substance of the invention may occur to person skilled in the art, the invention should be construed to include everything within the scope of the appended claims and equivalents thereof.

Claims

We Claim:
1. A method for sustainable reclamation of bio mass for obtaining carbon nanoparticles, the method comprising, obtaining the bio mass in powder form; subjecting the bio mass powder to an initial rapid heating from a temperature ranging from 100 °C to 600 °C for a predetermined first duration of time for removal of organic matter to obtain a residue; initiating a second slow heating step on the obtained residue for a predetermined second duration of time to obtain an intermediate; and cooling down the intermediate at a rate of 10 °C per minute to obtain carbon nanoparticles, wherein the method is performed under anaerobic conditions.
2. The method as claimed in claim 1 , wherein the predetermined first duration of time ranges from 20 minute to 70 minutes.
3. The method as claimed in claim 1 , wherein the second slow heating step comprises of heating upto a temperature in the range of 600 °C to 1000 °C at a rate of 5 °C/minute for a time duration of 40 minutes to 45 minutes.
4. The method as claimed in claim 1 , wherein the bio mass powder is obtained by first heating the bio mass at a temperature ranging from 80 °C to 100 °C followed by grinding and sieving the bio mass to obtain bio mass powder with grain size ranging from 50 to 100 urn. The method as claimed in claim 1 , wherein the heating of bio mass powder is carried out in a furnace in controlled temperature and anaerobic conditions wherein the anaerobic condition is maintained by continuous flow of an inert gas at rate of 100-150ml /cm3. The method as claimed in claim 1 , wherein the bio mass comprises of a plant based bio mass. The method as claimed in claim 1 , wherein the plant based bio mass is selected from a list comprising agricultural waste, fruit peels, vegetable peels, fruit seeds, palm leaves, palm nut, arecanut and plant leaves. The method as claimed in claim 1 , wherein the particle size of carbon nanoparticles ranges from 20 nm to 100 nm. The method as claimed in claim 1 , wherein the yield of carbon nanoparticles is in the range of 97% to 99%.
PCT/IN2023/050222 2022-03-09 2023-03-09 Sustainable reclamation of bio mass WO2023170708A1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013118150A1 (en) * 2012-02-08 2013-08-15 Council Of Scientific & Industrial Research "electronically conducting carbon and carbon-based material by pyrolysis of dead leaves and other similar natural waste"
EP3584217A1 (en) * 2009-03-26 2019-12-25 Northeastern University Carbon nanostructures from pyrolysis of organic materials

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3584217A1 (en) * 2009-03-26 2019-12-25 Northeastern University Carbon nanostructures from pyrolysis of organic materials
WO2013118150A1 (en) * 2012-02-08 2013-08-15 Council Of Scientific & Industrial Research "electronically conducting carbon and carbon-based material by pyrolysis of dead leaves and other similar natural waste"

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
HU ZHANGMAO, ZHOU TONG, TIAN HONG, FENG LEIHUA, YAO CAN, YIN YANSHAN, CHEN DONGLIN: "Effects of pyrolysis parameters on the distribution of pyrolysis products of Miscanthus", PROGRESS IN REACTION KINETICS AND MECHANISM, vol. 46, 1 January 2021 (2021-01-01), pages 146867832110109, XP093091331, ISSN: 1471-406X, DOI: 10.1177/14686783211010970 *
JIANGTAO ZHU ET AL.: "Synthesis of multiwalled carbon nanotubes from bamboo charcoal and the roles of minerals on their growth", BIOMASS AND BIOENERGY, vol. 36, 23 November 2011 (2011-11-23), pages 12 - 19, XP028346440, DOI: 10.1016/j.biombioe.2011.08.023 *
UDDIN M. N., TECHATO KUAANAN, TAWEEKUN JUNTAKAN, MOFIJUR M., RASUL M. G., MAHLIA T. M. I., ASHRAFUR S. M.: "An Overview of Recent Developments in Biomass Pyrolysis Technologies", ENERGIES, vol. 11, no. 11, pages 3115, XP093091330, DOI: 10.3390/en11113115 *

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