CHAPTER – II

2. Review of Literature

2.1. Green Chemistry

Green chemistry utilizes a set of principles which reduces or eliminates the use or

generation of hazardous substances in the design, manufacture and application of

chemical products. It seeks to reduce and prevent pollution at its source. In 1990 the

Pollution Prevention Act passed in the United States has helped to create a modus

operandi for dealing with pollution in an original and innovative way. It aims to avoid

problems before they happen and can be applied to organic chemistry, inorganic

chemistry, biochemistry, analytical chemistry, physical chemistry etc. When green

chemistry focuses on industrial applications, it emphasizes on minimization of hazard and

maximization of efficiency, the following images exposes that statement in detail [1-3].

4
2.2. Nanotechnology

Nanotechnology can be viewed as a combination of the existing sciences into the

nanoscale science. It is a new field of study, and the fate of nanoparticles in biological

and environmental systems is in general still unknown. Two main approaches are

generally dominant for manufacturing nanoparticles. One is the bottom up approach in

which the materials are built from their atomic or molecular counterparts which assemble

themselves chemically and physically by the principles of particular molecular

recognition. The other approach is the top-down, in which the nanoparticles are

constructed from larger entities without atomic level control. Examples of

nanotechnology in the modern world are designing of computer chip layouts based on

surface science as well as manufacturing of biosensors and drug delivery devices.

Nowadays nanoparticles are being used in real commercial applications such as

cosmetics, protective coatings and stain resistant clothes [4-6].

2.3. Green nanotechnology

Recently researchers are merging green chemistry and green engineering with

nanotechnology for a new field known as Green Nano for reduction of pollution at the

level of production. Green nanoscience/nanotechnology involves the application of green

chemistry principles to the design of nanoscale products, the development of

nanomaterial production methods and the application of nanomaterials. The approach

aims to develop an understanding of the properties of nanomaterials, including those

related to toxicity and ecotoxicity and to design nanoscale materials that can be

incorporated into high performance products that pose little hazard to human health or the
5
environment. It strives to discover synthesis/production methods that eliminate the need

for harmful reagents and enhance the efficiency of these methods, while providing the

necessary volume of pure material in an economically viable manner [7]. It also provides

proactive design schemes to ensure that the nanomaterials produced are inherently safer

by assessing the biological and ecological hazards in tandem with design. Finally, it seeks

applications of nanoscience that maximize societal benefit while minimizing impact on

the ecosystem. In this way, green nanoscience guides materials development, processing

and application design throughout the life cycle, starting with raw material selection to

end-of-life [8].

2.4. Application of Green Chemistry Principles to Nanoscience

Nanoparticles and other nanomaterials that exhibit size-dependent properties are

already finding application in products ranging from consumer healthcare goods to high

performance composites. In addition, a growing number of applications of

nanoscience/nanotechnology are being developed that promise environmental benefit.

Nearly all of the principles of green chemistry have been readily applied to the design of

nanoscale products, development of nanomaterials synthesis methods, and the application

of nanomaterials are depicted in Table 2.4. In nearly every case, several of the principles

can be applied simultaneously to drive the best design or solution [9].

6
Table 2.4: Principles of green chemistry in development of nanomaterials

7
2.5. Nanoparticles

Nanoparticles are larger than individual atoms and molecules but are smaller than

the bulk material. Since there is a size variation they do not obey neither the absolute

quantum chemistry nor the laws of classical physics and have properties that are very

different from that of the bulk material. There is no strict dividing line between

nanoparticles and non-nanoparticles. There is no particular definition for nanoparticles.

The internationally accepted definition is that any particle which has at least one

dimension less than 100nm is called a nanoparticle [10-12]. The following picture

explains about the nano in general visual scenery.

8
2.6. Synthesis of Nanoparticles

Nanoparticles are synthesized by various methods like gas phase and sol-gel

processing, sonochemical synthesis, cavitation processing, microemulsion processing and

high-energy ball milling. The different syntheses are as follows:

Solid and gas phase have some limitations such as difficulty in gathering the

products, expensive equipment, energy waste and environmental pollution. By

considering the above limitations we have preferred the liquid phase route i.e., sol–gel

process. Because of their high degree of monodispersity, surface modification, consistent

shape, they can be manipulated by dopant, surfactant, and capping agents [13-15].

2.6.1. Sol-gel Process

The sol-gel method is based on inorganic polymerization reactions. The sol-gel

process includes five different steps: hydrolysis, polycondensation, gelation, drying, and

9
thermal decomposition. Metal salts or metal alkoxides as the precursor are hydrolyzed

with water or alcohols according to the hydrolysis process

M(OR)x + mH2O → M(OR)x-m(OH)m + mROH

where if m is up to x, the reaction is total hydrolysis, followed by either a water or

alcohol as by product. In addition to water and alcohol, an acid or a base can also help to

hydrolyze the precursor. The synthesis of nanoparticles by sol-gel process is depicted in

Figure 2.6.1. Metal alkoxides are in general very reactive due to the presence of highly

electronegative OR- groups that stabilize the metal in its highest oxidation state and

render it very susceptible to nucleophilic attack. The lower electronegativity of transition

metals causes them to be more electrophilic and thus less stable towards hydrolysis,

condensation and other nucleophilic reactions. Controlling the conditions can be difficult

but successful control of the reaction conditions has the potential to produce materials of

consistent size, shape and structure [16-19].

Figure 2.6.1: Synthesis of nanoparticles by sol-gel process

10
2.7. Ionic liquids

Conventional synthesis of inorganic materials relies heavily on organic solvents.

Alternatively, the synthesis of inorganic materials in the presence of, ionic liquids (ILs)

represents a burgeoning direction in materials chemistry. Use of ionic liquids in solvent

extraction and organic catalysis has been extensively studied, but their use in inorganic

synthesis has just begun. Ionic liquids are a family of non-conventional molten salts that

can act as templates and precursors to inorganic materials, as well as solvents. They offer

many advantages, such as negligible vapour pressures, good thermal stability, tunable

solubility for both organic and inorganic molecules, and much synthetic flexibility. ILs

commonly defined as salts are liquid below 100oC. In 1914 Paul Warden observed that

Ethylammonium nitrate [EtNH3][NO3] have melting point of 13-14oC as first known

example for ILs. In the years to follow, very few examples built on Walden´s discovery

and it was not until the beginning of the next century that the science of ILs would take

its giant leap [20,21].

Most of the solvents employed for the synthesis of nanoparticles are highly toxic,

flammable and even explosive, the negative environmental and safety problems arising

through the use of volatile organic solvents can be defeated by a designer and greener

solvent which are termed as ionic liquids. They can be recovered and reused for next run

of the synthesis [22]. The general anions and cations of ionic liquids are as follows

(Fig. 2.7).

11
 Figure 2.7 General anions and cations of Ionic liquids

2.7.1. Why Ionic liquids are “Liquids”

Traditional salts like sodium chloride are able to pack efficiently pack to form a

crystal lattice. In ionic liquids; the cations are asymmetrically substituted with different

length groups to prevent the packing of the cations/anions into a crystal lattice [23].

Those lattice forms of both salts are in given below.

12
2.7.2. Applications of Ionic liquids

Because of their properties, ionic liquids attract great attention in many fields,

including organic chemistry, electrochemistry, physical chemistry, and engineering. In

addition, their non-volatility results in low impact on the environment and human health,

and they are recognized as solvents for "green chemistry." The following figures explain

the applications of ionic liquids in detail (Fig. 2.7.2 A), especially the importance of

imidazolium based ionic liquids in various fields (Fig. 2.7.2 B) [24, 25].

Figure 2.7.2 (A): Application of Ionic liquids

13
 Figure 2.7.2 (B): Imidazolium based ionic liquids in various applications

2.8. Biosynthesis of Nanoparticles

There are a large number of physical, chemical, biological, and hybrid methods

available to synthesize different types of nanoparticles. Although physical and chemical

methods are more popular in the synthesis of nanoparticles, the use of toxic chemicals

greatly limits their biomedical applications, particularly in clinical fields. Therefore,

development of reliable, nontoxic, and eco-friendly methods for synthesis of

nanoparticles is utmost importance to expand their biomedical applications. The

techniques for obtaining nanoparticles using naturally occurring reagents such as

vitamins, sugars, plant extracts, biodegradable polymers, and microorganisms as

reductants and capping agents could be considered as attractive concepts in

nanotechnology. These syntheses have led to the fabrication of limited number of

inorganic nanoparticles (mainly metal nanoparticles, although several metal oxides and

salts are also reported) [26-29].

14
 Biological entities and inorganic materials have been in constant touch with each

other ever since inception of life on the earth. Due to this regular interaction, life could

sustain on this planet with a well-organized deposit of minerals. Recently scientists

become more and more interested in the interaction between inorganic molecules and

biological species. Microorganisms can also be utilized to produce nanoparticles but the

rate of synthesis is slow and only limited number of sizes and shapes are amenable

compared to routes involving plant based materials [30-32].

2.8.1. Plants Extract Mediated Green Route for Biosynthesis of Nanoparticles

Among the reagents mentioned above, plant based materials seem to be the best

candidates and they are suitable for large-scale “biosynthesis” of nanoparticles. Plant

parts such as leaf, root, latex, seed, and stem are being used for metal nanoparticle

synthesis. The active key agents are believed to be polyphenols, present in tea, wine and

winery waste, red grape. Greener synthesis of nanoparticles provides advancement over

other methods as it is simple, cost effective, and relatively reproducible and often more

stable materials [33-35].

Phytomining is the use of hyper accumulating plants to extract a metal from soil

with recovery of the metal from the biomass to attain an economic profit. Hyper

accumulator species have a physiological mechanism that regulates the soil solution

concentration of metals. Exudates of metal chelates from root system will allow increased

flux of soluble metal complexes through the root membranes. It has been observed that

stress tolerant plants have more capacity to reduce metal ions to the metal nanoparticles.

15
Mechanism of biosynthesis of nanoparticles in plants may be associated with

phytoremediation concept in plants [36-38].

At present, fungi are gaining worldwide popularity as nano-factories for the green

synthesis of nanoparticles. Overall, biological materials provide an environmentally

friendly or greener chemical method to produce invaluable materials because the

biomaterial based routes eliminates the need to use harsh or toxic chemicals. There are

several reports on microbial and plant based synthesis of noble metal nanoparticles i.e.

gold, silver, platinum and palladium. However, the application of biological methods

using plant extract has not been exploited to synthesize semiconductor metal oxide

nanomaterials. Only few reports are available for the plant mediated synthesis metal

oxide nanoparticles. Titanium dioxide nanoparticles (100-150nm) have been prepared

from titanium isopropoxide solution using Nyctanthes leaves extract. Cubic In2O3

nanoparticles (5-50nm) were synthesized by a simple, cost effective and environmental

friendly route using indium acetylacetonate and Aloe vera plant extract solution. Highly

stable and spherical ZnO NPs have also been synthesized using Aloe vera extract.

Biosynthesis of magnesium oxide nanoparticles (MgO) was achieved by a novel, simple

green chemistry procedure using Nephelium lappaceum L peel extract as a precipitant and

capping agent [39-46].

16
2.9. Banana Stem

Banana stem (Cosmopolites sordidus) along with dietary fibers, proteins and

unsaturated fatty acids, banana flowers are also rich in vitamin E and flavanoids. They

are part of much cookery in the world. They also possess immense medicinal value. i.e

the tender core of the banana plant's trunk is an effective way to lose weight. People

suffering from kidney stones can have the extract prepared from the tender core of the

banana’s trunk as a remedy. It is diuretic in nature and helps to get rid of the toxins in the

body. It is also mild laxative and helps to cool the body.

Gold nanoparticles and bio-inspired palladium nanoparticles were synthesized

using banana peel extract (BPE) as a simple, non-toxic, eco-friendly 'green material'.

Boiled, crushed, acetone precipitated, air-dried peel powder was used to reduce palladium

chloride Banana peel extract mediated novel route for the synthesis of palladium

nanoparticles was also reported [47-50].

17
2.10. Metal oxide Nanopartricles

Metal oxides play a vital role in many areas of chemistry, physics and materials

science. The metal elements are able to form a large diversity of oxide compounds. These

can adopt a vast number of structural geometries with an electronic structure that can

exhibit metallic, semiconductor or insulator character. Oxide nanoparticles can exhibit

unique physical and chemical properties due to their limited size and high density of

corner or edge surface sites. In the emerging field of nanotechnology, a goal is to make

nanostructures or nanoarrays with special properties with respect to those of bulk or

single particle species [51].

2.10.1. Zinc oxide

It usually appears as a white powder and is nearly insoluble in water. Zinc oxide

(ZnO) is present in the earth crust as a mineral zincite and exists in different forms.

Among these the most important crystalline form is wurtzite phase of ZnO. The powder

is widely used as an additive for numerous materials and products including plastics,

ceramics, glass, cement, rubber, lubricants, paints, ointments, adhesives, sealants,

pigments, foods, batteries, ferrites, fire retardants, etc. ZnO is nontoxic and is compatible

with human skin making it a suitable additive for textiles and surfaces that come in

contact with human body. The increase in surface area of nanoscale ZnO compared to

bulk has the potential to improve the efficiency of the material function [52-54]. It is also

potentially used to treat leukemia and carcinoma cancer cell, strong antibacterial agent,

drug carrier and industrial sectors including environmental, synthetic textiles, food,

packaging, medical care, healthcare, as well as construction and decoration [55, 56].
18
2.10.2. Magnesium oxide

Magnesium oxide (MgO), or magnesia, is a white hygroscopic solid mineral that

occurs naturally as periclase and is a source of magnesium. It has an empirical formula of

MgO and consists of a lattice of Mg2+ ions and O2− ions held together by ionic bonds.

Magnesium hydroxide forms in the presence of water (MgO + H2O → Mg(OH)2), but it

can be reversed by heating it to separate moisture. There are few dense engineering

ceramics of the structural type made from pure magnesia. However there is a wide range

of refractory and electrical applications where magnesia is firmly established. The

properties of major interest are as follows, good refractoriness, good corrosion resistance,

high thermal conductivity, low electrical conductivity and transparency to infrared [57,

58]. Magnesia crucibles have found application in the alloy industry, nuclear industry and

chemicals industry where corrosion resistance is required. Magnesia (or Sorel) cement is

a refractory binder based on a magnesium oxychloride formulation. Magnesia powder is

widely used as a filling for electrical heating elements. Extruded magnesia protective

sheaths have been used to house thermocouples in aggressive environments. Magnesia

has been included in brake linings due to its thermo mechanical properties. Magnesia has

been used as a protective film for plasma display screens where its electro-optical

properties are used to advantage. High purity grades of magnesia have been used to grow

thin film semiconductors [59, 60].

19
2.11. Microorganism and Nanoparticles

It is well known that inorganic nanoparticles can act as antibacterial and

antifungal agents, and thus have the ability to interact with microorganisms. However,

prior to using microorganisms as a mean of transport for bioactive molecules, such as

nanoparticles or drugs linked to nanoparticles, it is essential to investigate how to deposit

the molecules within microorganisms. It has already been described how gram-negative

bacteria can be used for constructing bacterial ghosts, representing novel advanced

delivery and targeting vehicles suitable for the delivery of hydrophobic or water-soluble

drugs. Also, in pathogenic fungi, like C. albicans, several components associated with the

cell wall have been identified to play an important role in fungal–host interactions [61,

62].

2.11.1. Role of Bacteria cell wall

The bacterial cell wall is designed to provide strength, rigidity, and shape, and to

protect the cell from osmotic rupture and mechanical damage. According to their

structure, components, and functions, the bacteria cell wall can be divided into the two

main categories: Gram positive (+) and gram negative (–). The wall of gram-positive

cells contains a thick layer (i.e., 20–50nm) of peptidoglycan (PG), which is attached to

teichoic acids that are unique to the gram-positive cell wall (Fig. 2.11.1). We have opted

these for two types of pathogenic bacteria because the following reasons -E. coli: Gram-

negative bacteria, virulent strain causes food poisoning, urinary tract infection and

neonatal meningitis [63].

20
Figure 2.11.1: Bacterial cell structure. (a) Gram-positive (b) Gram-negative

bacterial

The cell wall of gram-negative bacteria is structurally and chemically more

complex. It comprises a thin PG layer and an outer membrane, over the surface

membrane. The outer membrane of gram-negative bacteria often confers resistance to

hydrophobic compounds including detergents and contains as a unique component,

lipopolysaccharide, which increase the negative charge of cell membranes and are

essential for structural integrity and viability of the bacteria [64].

21
2.11.2. Antibacterial Activity of ZnO Nanoparticles

Antibacterial agents are broadly of two types, organic and inorganic. At high

temperatures/pressures organic antibacterial materials are found to be less stable

compared to inorganic antibacterial agents. ZnO nanoparticles showed greater

antibacterial activity apparently than micro particles. The exact mechanisms of the

antibacterial action have not yet been clearly identified. ZnO particles have bactericidal

effects on both gram-positive and gram-negative bacteria [65]. They even have

antibacterial activity against spores which are resistant to high temperature and high

pressure. From the literature it is evident that the antibacterial activity of ZnO

nanoparticles depends on the surface area and concentration, while the crystalline

structure and particle shape have little effect. Further it is also mentioned in the literature

that smaller size and larger surface area of the ZnO nanoparticles are good its

antibacterial activity [66].

Some researchers have proposed in their study that the generation of hydrogen

peroxide is the main factor of the antibacterial activity, while it also indicated that the

binding of the particles on the bacteria surface due to the electrostatic forces could be

another factor. The previous investigation on the antibacterial activity of ZnO particles

against pathogenic bacterial species like Escherichia coli, Pseudomonas aeruginosa,

Bacillus subtilis, and Streptococcus pneumonia have been reported [67]. Moreover, ZnO

is a safe reagent to humans and animals, which could be an ideal potential antibacterial

reagent to replace some antibiotics. However, few studies have been conducted to

evaluate the antibacterial effects of zinc oxide nanoparticles on E. coli K88 [68].

22
2.11.3. Antibacterial Activity of MgO Nanoparticles

The antibacterial activities of magnesium oxide nanoparticles (MgO NPs) alone

or in combination with other antimicrobials against E. coli O157:H7 and Salmonella

Stanley were investigated. These results suggest that MgO NPs alone or in combination

with nisin could potentially be used as an effective antibacterial agent to enhance food

safety [69]. Antibacterial activity of MgO NPs was evaluated against the gram-negative

bacteria Escherichia coli and Pseudomonas aeruginosa as well as the gram-positive

bacterium Staphylococcus aureus by microtitre plate-based assay incorporating resazurin

as an indicator of cell growth. It was suggested that the mechanism of the antibacterial

activity of the MgO NPs relied on the presence of defects or oxygen vacancy at the

surface of the nanoparticle which led to the lipid peroxidation and reactive oxygen

species generation [70].

Antibacterial activity of the metal oxide nanoparticles against chosen antibiotic

resistant bacterial pathogens was investigated. It reveals that, all the nanoparticles

showed antibacterial activity against Pseudomonas aeruginosa and Streptococcus

pneumoniae. Of these, MgO nanoparticle showed maximum sensitivity [(16.00, 0.53)

mm dia] against Streptococcus pneumonia [71]. The zone of inhibition was found to

more for gram positive bacteria compared with gram negative bacteria. Antibacterial

property of prepared nanoparticles is decreases with increases of calcinations

temperature, i.e., it depends upon the size of the nanoparticles [72]. Our study was

undertaken to investigate the antibacterial activity of ZnO and MgO nanoparticles against

S.aureus and E. coli.

23
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29
 Aim and Scope

 Synthesize of well-defined nanostructures of ZnO and MgO by greener route using

eco-friendly ionic liquids [BMIM BF4, EMIM BF4 and BMIM PF6] as solvent

(Chapter 4 & 6).

 Study the role of calcination temperature on the structure and size of ZnO and MgO

nanostructures in BMIM BF4 ionic liquid. Comparison of effect of calcination

temperature on ZnO and MgO nanostructures in conventional and ionic liquid solvent

(Chapter 5 & 7).

 Biosynthesis of ZnO and MgO nanostructures using banana stem extract without

addition of any conventional hydrolytic agent. Study the distinct role of ionic liquid in

biosynthesize of ZnO and MgO using banana stem extract (Chapter 8 & 9).

 The influence of ionic liquids and temperature on the surface morphology, crystalline

parameters and size of ZnO and MgO nanoparticles was studied by powder X-ray

diffraction, Scanning electron microscopy, Particle size analyser and Transmission

electron microscope. The antibacterial activity of the ZnO and MgO nanoparticles

obtained in three different ionic liquids and hydrolyzing agent were evaluated by agar

diffusion test against S.aureus and E.coli bacteria.

 The influence of the physicochemical properties of IL and banana stem extract on

the growth of the nanostructures is inquired with the help of FT-IR, EDX and TGA

analysis. These findings explicit the differences in reactivity and thus gauge the

important parameters to consider when carrying out in ionic liquid media.

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