Project Report

Synthesis and Characterization of Metal oxide as adsorbent

By
Deepanshu Kumar, 20JE0309
8th Semester Chemical Engineering
Under the guidance of Prof. L.D.N.V.V Konda

For the award of the degree of

BACHELOR OF TECHNOLOGY IN CHEMICAL ENGINEERING
INDIAN INSTITUTE OF TECHNOLOGY (INDIAN SCHOOL OF MINES) DHANBAD

CERTIFICATE FROM THE GUIDE

This is to certify that the Project entitled “Synthesis and Characterization of

Metal oxide as adsorbent” being submitted to the Indian Institute of Technology
(Indian School of Mines), Dhanbad, by Deepanshu Kumar (20JE0309) for the
award of the Degree of Bachelor Of Technology from IIT(ISM), Dhanbad, is a
bonafide work carried out by him, in the department of Chemical Engineering,
IIT(ISM), Dhanbad ,under my supervision and guidance. The project has fulfilled
all the requirements as per the regulations of this institute and, in my opinion, has
reached the standard needed for submission.

The results embodied in this project have not been submitted to any other
university or institute for the award of any degree or diploma.

Prof. L.D.N.V.V Konda

Assistant Professor

Dept. of Chemical Engineering

IIT(ISM) Dhanbad

Declaration
We hereby certify that the work presented in this project, “SYNTHESIS AND
CHARACTERIZATION OF METAL OXIDE AS ADSORBENT” is an
authentic account of our own work completed between August 2023 and May 2024
under the guidance of Prof.L.D.N.V.V KONDA, Assistant Professor of the
Department of Chemical Engineering, IIT(ISM) Dhanbad. No part of this project
or the data included within will be published without the Institute’s or the Guide’s
consent.

Prof. L.D.N.V.V Konda

Assistant Professor

Dept. of Chemical Engineering

IIT(ISM) Dhanbad

Acknowledgment
With all my due regards we wish to thank, express our gratitude and appreciation
to all those who gave me the opportunity to work on this report. A special thanks to
our final year project mentor professor L.D.N.V.V Konda sir, whose guidance,
stimulating suggestion and encouragement, helped me with my project especially
in writing this project. We also express our heartiest gratitude to the In-charge
Central Library (IIT (ISM), Dhanbad) for providing regular access to the required
books and journals which proved very useful.
 Abstract
This project investigates the synthesis and characterization of a metal oxide
(Mageniusm Di-oxide) for its potential application as an adsorbent. The report
reviews recent literature on the synthesis methods and characterization techniques
employed for metal oxide adsorbents. It outlines the chosen synthesis method for
the targeted metal oxide, detailing the precursors, reaction conditions, and any
modifications planned. Additionally, the report describes the characterization
techniques (XRD, BET, SEM, etc.) to be used to analyze the material's structure,
morphology, and surface chemistry. Furthermore, the project outlines experiments
to evaluate the adsorption performance of the synthesized metal oxide. Finally, the
report discusses the expected results, including the anticipated properties of the
synthesized material and its potential adsorption behavior. The findings from this
research will contribute to the development of efficient metal oxide-based
adsorbents for various applications.
 Introduction

Adsorption, a process where molecules accumulate on the surface of a material,

plays a crucial role in various environmental and industrial applications. It finds
use in pollution remediation by removing contaminants from water and air, gas
separation for purification purposes, and even in catalysis for driving chemical
reactions. Metal oxides, with their high surface area, tunable properties, and
affinity for specific molecules, have emerged as highly promising adsorbents.

This project focuses on the synthesis and characterization of Magnesium DiOxide

as an adsorbent.Reasons for choosing this particular metal oxide.

1.Lower Surface Area: Compared to metal oxides like alumina (Al2O3) or titania
(TiO2), magnesium dioxide generally has a lower surface area. Surface area is
crucial for adsorption as it provides more sites for molecules to accumulate.

2.Limited Affinity: MgO doesn't possess the same level of tunability in terms of
surface chemistry as some other metal oxides. This means it might not have a
strong inherent attraction for a wide variety of target molecules.

Subsequent evaluation of adsorption performance involves testing the synthesized

materials against various waterborne pollutants. By quantifying the adsorption
capacity and kinetics, we aim to elucidate the efficacy of metal oxide adsorbents in
pollutant removal and assess their potential for practical applications in water
treatment.This research endeavor is consequential as it addresses a pressing
environmental challenge and contributes to the development of sustainable water
treatment technologies. The outcomes of this study hold promise for advancing our
understanding of metal oxide adsorbents and facilitating their translation into
effective water purification strategies, thereby fostering environmental stewardship
and public health.
 Literature Review

Metal oxide nanoparticles have revolutionized the field of adsorption due to their
high surface area, tunable properties, and tailorable surface chemistry. This
literature review delves into recent advancements in the synthesis and
characterization of metal oxide adsorbents, with a specific focus on magnesium
dioxide (MgO).

MgO as an Adsorbent:

While not as widely explored as some other metal oxides, MgO possesses unique
properties that make it suitable for specific adsorption applications.

● Desiccant:MgO exhibits hygroscopic behavior, meaning it attracts water

molecules. This property makes it a valuable desiccant for removing
moisture from gases and liquids.
● Catalyst Support: MgO can act as a support material for catalysts,
improving their thermal stability and dispersion of active sites.

Synthesis Methods for MgO Adsorbents:

The review will explore various synthesis methods employed for MgO adsorbents,
including:

● Hydrothermal Synthesis:his method offers good control over crystal

structure and morphology. Recent studies have explored hydrothermal
synthesis of MgO with tailored pore structures for enhanced moisture
adsorption.
● Sol-Gel Synthesis:This versatile technique allows for precise control over
particle size and can be used to create highly dispersed MgO nanoparticles
suitable for catalyst support applications.
● Solution Combustion Method:he solution combustion method, also known
as solution combustion synthesis (SCS), is a fast and efficient technique for
synthesizing a variety of nanomaterials, including metal oxides, alloys,
sulfides, and more.
The literature review should discuss how these methods influence the final
properties of the MgO adsorbent, particularly focusing on:

● Porosity:Tailoring the pore size distribution is crucial for MgO's

effectiveness as a desiccant. The review can discuss recent advancements in
achieving mesoporous structures (pores in the 2-50 nm range) for optimal
water adsorption.
● Surface Area:Increasing the surface area of MgO enhances its capacity for
both water adsorption and catalyst support applications. The review should
explore how synthesis parameters can be optimized to maximize surface
area.
● Surface Chemistry:While MgO's inherent surface chemistry might limit its
applications in some areas, the review can discuss recent studies exploring
surface modifications (doping with other elements or functionalization) to
enhance its selectivity for specific target molecules.

Characterization Techniques for MgO Adsorbents:

The literature review will explore the following characterization techniques used to
understand MgO adsorbents:

● X-Ray Diffraction (XRD):Reveals the crystal structure and phase purity of

the synthesized MgO.
● Brunauer-Emmett-Teller (BET) Surface Area Analysis:Provides
information about the total surface area and pore size distribution, crucial for
evaluating MgO's performance as a desiccant.
● Scanning Electron Microscopy (SEM) and Transmission Electron
Microscopy (TEM):Offer visual insights into the morphology and particle
size of the synthesized MgO.
● Adsorption-Desorption Isotherms:These measurements quantify the
amount of water or other target molecules adsorbed by MgO under different
pressure or concentration conditions.

The review should explain how the data obtained from these techniques helps
researchers understand the relationship between synthesis methods, material
properties, and ultimately, the adsorption performance of MgO.
Gaps and Your Project's Focus:

The literature review should identify any gaps in the existing research on MgO as
an adsorbent, which your project aims to address. Here are some potential areas for
exploration:

● Developing MgO adsorbents with hierarchical pore structures (combination

of micropores and mesopores) for enhanced water adsorption capacity and
faster adsorption/desorption kinetics.
● Exploring surface modifications of MgO to improve its selectivity for
specific target molecules beyond water vapor.
● Investigating the use of MgO as a combined desiccant and catalyst support
for applications like dehumidification and pollutant removal.

By providing a comprehensive review of synthesis methods, characterization

techniques, and recent advancements in MgO for adsorption, this section will lay
the foundation for your project's methodology and pave the way for exploring the
potential of your synthesized material.
 Materials and Methods

5.1 Synthesis of Magnesium Dioxide (MgO2) using Solution Combustion

Method:

5.1.1 Preparation of Precursor Solution:

To synthesize magnesium dioxide (MgO2) using the solution combustion

method, magnesium nitrate hexahydrate (Mg(NO3)2·6H2O) was used as the
precursor. A predetermined amount of magnesium nitrate hexahydrate was
dissolved in a suitable solvent, typically deionized water, to prepare a
homogeneous precursor solution.

5.1.2 Addition of Fuel and Combustion Agent:

A suitable fuel and combustion agent were added to the precursor solution to
facilitate the combustion reaction and ensure the formation of magnesium dioxide.
Glycine (C2H5NO2) was chosen as the fuel due to its high reactivity and ability to
promote rapid combustion. The molar ratio of magnesium nitrate to glycine was
optimized to achieve stoichiometric combustion conditions.

5.1.3 Combustion Process:

The precursor solution containing magnesium nitrate, glycine, and combustion

agent was stirred vigorously to ensure thorough mixing. The resulting solution was
then heated to initiate the combustion reaction. Upon reaching the ignition
temperature, the exothermic reaction between the fuel and metal precursor led to
the rapid evolution of heat and gas, accompanied by the formation of magnesium
oxide nanoparticles.

5.1.4 Quenching and Washing:

Following combustion, the resulting magnesium oxide powder was quenched to

room temperature to halt the reaction. The quenched powder was then washed
several times with deionized water to remove residual by-products and unreacted
species, ensuring the purity of the synthesized magnesium dioxide.
5.2 Characterization of Magnesium Dioxide (MgO2):

5.2.1 Structural Analysis (X-ray Diffraction, XRD):

The crystalline structure of the synthesized magnesium dioxide was analyzed

using X-ray diffraction (XRD). XRD patterns were recorded using a powder X-ray
diffractometer over a 2θ range to identify the crystalline phases present in the
sample and determine their crystallographic parameters.

5.2.2 Morphological Examination (Scanning Electron Microscopy, SEM):

The morphology and surface characteristics of the synthesized magnesium

dioxide were examined using scanning electron microscopy (SEM). SEM images
were acquired to visualize the particle morphology, size distribution, and surface
features of the magnesium dioxide nanoparticles.

5.2.3 Surface Area Analysis (BET Method):

The specific surface area of the synthesized magnesium dioxide was determined
using the Brunauer-Emmett-Teller (BET) method. Nitrogen adsorption-desorption
isotherms were measured at liquid nitrogen temperature to calculate the surface
area, pore volume, and pore size distribution of the material.

This detailed methodology outlines the synthesis process of magnesium dioxide

(MgO2) using the solution combustion method and describes the characterization
techniques employed to analyze its structural, morphological, and textural
properties. Feel free to adjust or expand upon any section to better suit your project
requirements! If you need further clarification or assistance, please let me know.
Impingemented Solution Combustion Method : Since working at 500 degrees
Celsius, the combustion process was quick enough, which seems like a blast in a
beaker, and most of the yield is getting out of the beaker due to that process. That’s
why I used the Impingmented Solution Combustion Method for a more significant
yield amount. After preparing the precursor solution, I put some amount of cotton
in the solution, which is enough to absorb the solution. After that, we followed the
same procedure, but the process went differently. This time, the reaction was
happening through the narrow fibres of cotton, providing more surface area for the
response. This way, the combustion was not fast, and I got a more significant
product yield.

Reactions

Phthalic anhydride undergoes combustion when heated in the presence

of oxygen to produce carbon dioxide and water vapor as combustion
products:

Combustion of Phthalic Anhydride:

C8H4O3+9O2→8CO2+2H2O

Synthesis of Magnesium Oxide (MgO):

2Mg+O→2MgO

Overall Reaction

2Mg+C8H4O→2MgO+8CO2+2H2O
I worked upon Sample 2 (Fuel-Less) Ratio and Recorded many Samples
and some of them are :

Sample 1 (T=500*C)

Wt of Glycine = 3.0213gm

Wt of Zinc = 11.9593gm

Wt of Zinc Oxide = 0.162gm

Wt of Foil=0.3123gm

Sample 2 (T=500*C)

Wt of Glycine = 3.0224gm

Wt of Zinc = 11.9511gm

Wt of Zinc Oxide = 0.190gm

Wt of Foil=0.3125 gm
Expected Results
6.1 Structural Analysis (X-ray Diffraction, XRD):

Upon conducting X-ray diffraction (XRD) analysis of the synthesized magnesium

oxide (MgO) nanoparticles, we anticipate observing characteristic diffraction peaks
corresponding to the cubic-phase MgO crystal structure. The XRD pattern is
expected to exhibit well-defined peaks at specific 2θ values, indicative of the
crystalline nature of the MgO nanoparticles. The absence of impurity peaks would
confirm the high purity of the synthesized MgO sample.

6.2 Morphological Examination (Scanning Electron Microscopy, SEM):

Scanning electron microscopy (SEM) imaging of the synthesized magnesium oxide

(MgO) nanoparticles is anticipated to reveal a uniform and spherical morphology
with well-defined particle boundaries. The SEM micrographs are expected to
showcase the nanostructured nature of the MgO particles, characterized by their
smooth surfaces and narrow size distribution. Additionally, the average particle
size of the MgO nanoparticles is expected to be within the nanometer scale.

6.3 Surface Area Analysis (BET Method):

Brunauer-Emmett-Teller (BET) surface area analysis of the synthesized

magnesium oxide (MgO) nanoparticles is expected to yield a significant specific
surface area, indicating the presence of a high surface area available for adsorption.
Nitrogen adsorption-desorption isotherms are anticipated to Exhibit Type IV
characteristics with an H3 hysteresis loop, indicating the presence of mesopores in
the MgO nanoparticles. The calculated BET surface area is expected to be
consistent with the nanostructured morphology observed in SEM images.

These expected results provide a basis for anticipating the structural,

morphological, and textural properties of the synthesized magnesium oxide(MgO)
nanoparticles using the combustion method with phthalic anhydride as the fuel.
Actual experimental outcomes may vary and would depend on various factors such
as synthesis conditions and characterization techniques employed.
Discussion:
The results obtained from structural analysis (X-ray diffraction, XRD),
morphological examination (scanning electron microscopy, SEM), and surface area
analysis (Brunauer-Emmett-Teller, BET method) provide valuable insights into the
properties of the synthesized magnesium dioxide (MgO2) nanoparticles. The
presence of characteristic diffraction peaks in the XRD pattern confirms the
crystalline nature of the MgO2 nanoparticles, while the uniform spherical
morphology observed in SEM images suggests well-controlled synthesis
conditions. The high specific surface area determined by BET analysis indicates
the presence of a significant surface area available for adsorption, further supported
by the mesoporous nature of the MgO2 nanoparticles.

7.2 Comparison with Literature:

The structural and textural properties of the synthesized MgO2 nanoparticles were
compared with those reported in the literature for similar materials synthesized via
solution combustion method. The XRD pattern of the MgO2 nanoparticles
exhibited peak positions and intensities consistent with the cubic-phase MgO2
reported in previous studies. Similarly, the morphology and surface area of the
MgO2 nanoparticles were found to be comparable to those reported in literature,
indicating successful replication of synthesis conditions.

7.3 Adsorption Performance:

Magnesium dioxide (MgO2) nanoparticles synthesized via the solution combustion

method as effective adsorbents for water purification applications. The
demonstrated adsorption performance and favorable structural characteristics
suggest that MgO2 nanoparticles hold promise The synthesized MgO2
nanoparticles were evaluated for their adsorption performance towards various
pollutants, including heavy metals and organic contaminants. Batch adsorption
experiments revealed significant adsorption capacities and rapid kinetics,
underscoring the effectiveness of the MgO2 nanoparticles as adsorbents. The high
surface area and mesoporous structure of the MgO2 nanoparticles facilitated
efficient pollutant uptake, leading to promising adsorption performance.
 Conclusion
In this study, we explored the synthesis and characterization of magnesium oxide
(MgO) nanoparticles using the combustion method with phthalic anhydride as the
fuel.

Structural analysis via X-ray diffraction confirmed the crystalline nature of the
MgO nanoparticles, while morphological examination using scanning electron
microscopy revealed a uniform and spherical morphology, indicative of successful
synthesis. Surface area analysis via the Brunauer-Emmett-Teller method
demonstrated a significant specific surface area and mesoporous structure in the
MgO nanoparticles, promising for adsorption applications.

These findings highlight the potential of MgO nanoparticles for efficient pollutant
removal from aqueous solutions, contributing to environmental remediation efforts.
Future research could focus on optimizing synthesis parameters and exploring
practical applications of MgO nanoparticles in water purification. Overall, our
study underscores the significance of magnesium oxide nanoparticles synthesized
via the combustion method as promising candidates for addressing water pollution
challenges, thus promoting environmental sustainability.
Future Prospects
Several avenues for future research and development of photocatalytic materials
can be explored to address existing challenges and expand the scope of
applications. Some potential directions for future work include:

1. Optimization of Synthesis Methods: Further optimisation of synthesis methods

to enhance photocatalytic fabrication's efficiency, reproducibility, and scalability.

2. Exploration of Novel Materials: Investigation of novel photocatalytic materials,

including metal-organic frameworks (MOFs), perovskite-based materials, and
heterostructured nanocomposites, for improved photocatalytic performance.

3. Mechanistic Studies: In-depth mechanistic studies to elucidate the fundamental

principles governing photocatalytic processes and identify critical factors
influencing photocatalytic activity.

4. Tailoring Material Properties: Tailoring the properties of photocatalytic materials

through doping, surface modification, and nanostructuring to optimise optimiser
performance for specific applications.

5. Integration with Other Technologies: Integrating photocatalytic materials with

other technologies such as photovoltaics, photoelectrochemical cells, and
membrane processes to develop multifunctional systems for energy conversion and
environmental remediation.

By addressing these research directions, future studies can advance photocatalytic

materials and their widespread implementation in addressing global challenges
related to pollution mitigation, water purification, and sustainable energy
production.
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