Chapter 3. Nano Technology in Industrial Wastewaters Treatment

Novel Technology for
Industrial wastewater
Xiang-fei Lyu
Chapter 3. nano technology in Industrial
Wastewaters Treatment Part Ⅰ
Contents
 3.1 Introduction to nanotechnology

 3.2 Development of nanotechnology in industrial
wastewaters Treatment
 3.3 Synthesis techniques of nanomaterials (including
case study)
 3.4 Performance of nanomaterials in heavy metals
removal
3.1 Introduction to nanotechnology
3.1.1 WHAT IS NANOMETER SCALE?
In 1959, Physics Nobel Laureate Richard Feynman gave a talk at

California Institute of Technology on the occasion of the
American Physical Society meeting. The talk was entitled
‘There’s Plenty of Room at the Bottom’. Although Feynman could
not predict it, this lecture was to become a central point in the
field of nanotechnology, long before any thing related with the
word nano had emerged. The term nano derives from the Greek
word for dwarf. It is used as a prefix for any unit such as a
second or a meter, and it means a billionth of the unit. Hence, a
nanometer (nm) is a billionth of a meter, or 10−9 meters. To get
a perspective of the scale of a nanometer, please see a length
scale showing the nanometer context in Figure 3.1. The
nanometerscale is commonly indicated as 1–100 nm, but
nanoscience and nanotechnology often deals with objects bigger
than 100 nm.
3.1.2 WHAT IS A NANOMATERIAL?
Nanoscale materials are defined as a set of substances where at

least one dimension is less than approximately 100 nanometers. A
nanometer is one millionth of a millimeter, approximately 100,000
times smaller than the diameter of a human hair. Nanomaterials are
of interest because at this scale unique optical, magnetic,
electrical, and other properties emerge.
Materials in the nanometer

scale may exhibit physical
properties distinctively
different from that of the
bulk. The two main reasons for
this change in behaviour are an
increased relative surface area,
and the dominance of quantum
effects.
Figure 3.1 The nanoscale.
3.1.3 DEFINITION OF NANOSCIENCE AND NANOTECHNOLOGY
Nanoscience is similar to materials science in that it is an integrated

convergence of academic disciplines. There exist a couple of major
distinctions between the two: size and biology. The objects are
controlled on this size scale either in terms of manufacturing,
modification or analysis, and the research includes some aspect of
novelty either in terms of material studied, methods used or questions
asked.
According to Royal Society of Chemistry, Nanotechnology is defined
as ‘Nanotechnologies are the design, characterization, production and
application of structures, devices and systems by controlling shape and
size at nanometre scale’. Nanotechnology is a enabling convergent
technology that cuts across all vertical industrial sectors while
nanoscience is a horizontal integrating interdisciplinary science that
cuts across all vertical science and engineering disciplines.
Nanotechnology is a disruptive technology with a high barrier of
entry that will impact the development of enhanced materials and
devices.
3.1.4 HISTORY OF NANOTECHNOLOGY
The Egyptians used ink containing

nanoparticles of black pigment.
Nanoparticles of lead sulfide were

used by the Romans to dye their
hair black.
Nanoparticles of gold and silver have

also been used since the 10th century
to color ceramics and stained glass.
3.1.4 HISTORY OF NANOTECHNOLOGY
 The first mention of nanotechnology (not yet using that

name) was in a talk given by Feynman (1959), entitled ‘Theres
Plenty of Room at the Bottom’.
 The first use of the term ‘nanotechnology’ was by Taniguchi
(1974) at the International Conference on Precision
Engineering (ICPE).
 Ideas of nanotechnological strategy, which were put forward
by Feynman, were developed by E. Drexler in his book
‘Vehicles of creation: the arrival of the nanotechnology
era’ (1986).
 The 1986 Nobel Prize in Physics was awarded to Gerd Binnig
and Heinrich Rohrer to honor their design of the scanning
tunneling microscope (STM). nanomaterials scientist.
3.1.5 CLASSIFICATION OF NANOSTRUCTURED MATERIALS
There are several ways to classify nanomaterials. This depends very

much on the applications and philosophy which are adopted. We shall
just present here two extreme classifications which can be found in
the literature. In the first one, the focus will be on the composition of
the material. The most current nanomaterials could be organized into
four types depending on composite of nanomaterials:
(1) Carbon Based Materials
(2) Metal Based Materials
(3) Dendrimers
(4) Composites
(1) Carbon Based Materials

These nanomaterials are composed mostly of carbon, most commonly
taking the form of a hollow spheres, ellipsoids, or tubes. Spherical
and ellipsoidal carbon nanomaterials are referred to as fullerenes,
while cylindrical ones are called nanotubes. These particles
havemany potential applications, including improved films and
coatings, stronger and lighter materials, and applications in
electronics. This classification includes fullerenes, carbon
nanotubes, graphene and the likes.
(2) Metal Based Materials
These nanomaterials include quantum dots, noblemetal nanomaterials
and metal oxides, such as zinc oxide. A quantum dot is a closely
packed semiconductor crystal comprised of hundreds or thousands
of atoms, and whose size is on the order of a few nanometers to a
few hundred nanometers. Changing the size of quantum dots
changes their optical properties. For example, titanium dioxide
(TiO2) nanoparticles are extensively used in applications such as
paint, sunscreen, and toothpaste.
(3) Dendrimers
These nanomaterials are nanosized polymers built from branched units.
The surface of a dendrimer has numerous chain ends, which can be
tailored to perform specific chemical functions. This property could
also be useful for catalysis. Also, because three-dimensional
dendrimers contain interior cavities into which other molecules could
be placed, they may be useful for drug delivery.
(4) Composites
Composites combine nanoparticles with other nanoparticles or with
larger, bulk-type materials. Nanoparticles, such as nanosized clays, are
already being added to products ranging from auto parts to packaging
materials, to enhance mechanical, thermal, barrier, and flame-
retardant properties.
Another classification has the focus on the macroscopic dimensions of the
material. This is shown schematically in Figure 3.2.
Figure 3.2 Classification of materials according to the dimensionality of the nanostructures.

3.1.6 UNIQUE PROPERTIES OF NANOMATERIALS
The unique properties of these various types of intentionally
produced nanomaterials give them novel electrical, catalytic,
magnetic, mechanical, thermal, or imaging features that are highly
desirable for applications in commercial, medical, military, and
environmental sectors. These materials may also find their way into
more complex nanostructures and systems. As new uses for materials
with these special properties are identified, the number of products
containing such nanomaterials and their possible applications continue
to grow.
Some known physical properties of nanomaterials are related to
different origins: for example, (i) large fraction of surface atoms, (ii)
large surface energy, (iii) spatial confinement, and (iv) reduced
imperfections.
3.2 Development of nanotechnology in
industrial wastewaters Treatment
These newly discovered properties of nano-scale materials have
opened up exciting fields of study and applications in areas that can
improve the quality of human life in the fields of water and health. Use
of nanotechnology in water and wastewater treatment, not only shows
its capacity to overcome different challenges associated with
conventional technology but also explore novel treatment technology to
treat and reuse of wastewater in respect of economic feasibility and
water quality standard.
In this section, an overview of recent advances in nanotechnology for
water and wastewater treatment is discussed here. The application of
nanomaterials in wastewater is critically discussed in perspective of
their functional processes. Moreover, the challenges associated with
the application of nanotechnology towards full-scale wastewater
treatment also are discussed here.
3.2.1 Recent application of nanotechnology in water and
wastewater treatment
Since water treatment by using nanoparticles has potential for

application, however, its usage cost should be managed in ways to
survive existing competition in the market.
Due to higher surface to volume ratio they impart size dependent
properties such as high reactivity, higher adsorption capacity, and
higher dissolution activity can be used in wastewater treatment. In
addition to that some unique property like superparamagnetism,
semiconducting, and quantum confinement effect also added
advantages in treatment processes.
3.2.1 Recent application of nanotechnology in water and
wastewater treatment
There are various recent advances on different nanomaterials
(nanostructured catalytic membranes, nanosorbents, nanocatalysts,
bioactive nanoparticles, biomimetic membrane and molecularly imprinted
polymers (MIPs)) for removing toxicmetal ions, disease causingmicrobes,
organic and inorganic solutes from water (Figure 3.3).
Fig. 3.3 Application of nanotechnology in wastewater treatment.

3.2.2 Adsorption
Sorbents are widely used in tertiary treatment and purification of
wastewater and water to remove organic and inorganic contaminants.
Efficiency of conventional sorbents which are used in adsorption
processes such as activated carbon, ion-exchange resins and so on.
suffer due to lack of high available surface area or active sites, lack
of selectivity and specificity, and lack of adsorption kinetics.
The use of nanomaterials (Nanosorbent) may have advantages to
overcome challenges of conventional materials (Sorbents) due to the
much larger surface area of nanoparticles, higher specificity and
selectivity, and tunable pore size and surface chemistry on a mass
basis. In addition, the unique structure and electronic properties of
some nanoparticles can make them especially powerful adsorbents.
Commercialized nanosorbents are very few mainly from the U.S. and
Asia but research is on going on in large numbers targeting various
specific contaminants in water.
3.2.2.1 Carbon nanotubes in waste water treatment
Discovery of carbon nanotubes (CNTs) eventually revolutionize the
future nanotechnologies area. CNTs are seamless cylinder-shaped
macromolecules with a radius as small as a few nanometers, and up to
several micrometers in length.
CNTs embedded nanotechnologies have found water-treatment
applications in many fields, such as sorbents, catalyst, filters or
membranes. In aqueous phase, CNTs get aggregated due to
hydrophobic nature and help in forming spaces and grooves for
adsorption of organic molecules. This property has attracted a lot of
attention as very powerful adsorbents for a wide variety of organic
compounds from water
For the removal of metals and other inorganic ions, mainly nanosized
metal oxides but also natural nanosized clays have been investigated.
Also, oxidized and hydroxylated CNTs are good adsorbers for metals.
Fig. 3.4 Common applications of metal

oxide nanoparticles.
Fig. 3.5 Five types of metal

oxide nanoparticles.
3.2.2.2 Metal nanomaterials in wastewater treatment
Nanoparticles formed by metal or metal oxides are another type of

inorganic nanomaterials, which are used broadly to remove heavy
metal ions in wastewater treatment. Nanosized metals or metal oxides
include nanosized silver nanoparticles, ferric oxides, titanium oxides,
magnesium oxides, copper oxides, cerium oxides, and so on, all these
provide high surface area and specific affinity. Besides, common
metal oxides possess little environmental impact due to low solubility
and thus, no secondary pollution; they have been adopted as sorbents
to remove heavy metals.
Recently, there have been several reports on magnetic oxides,

especially Fe3O4, being used as nano- adsorbents for the removal of
various toxic metal ions from wastewater, such as Ni2+, Cr3+, Cu2+, Cd2+,
Co2+, Hg2+, Pb2+, and As3+
3.2.3 Photocatalysis in wastewater treatment
Photo-catalyst activated by UV lights can oxidize organic

pollutants into non-toxic products, such as carbon dioxide, water and
can also disinfect certain bacteria. Photo-Catalysis is defined as
‘acceleration of photoreaction in presence of a catalyst’. A catalyst
does not change in itself or get consumed in the chemical reaction.
Figure 3.4 Schematic diagram of photocatalysis.

In catalyzed photolysis, light is absorbed by an adsorbed
substrate. In photo generated catalysis the photo catalytic
activity (PCA) depends on the ability of the catalyst to create
electron-hole pairs, which generate free radicals (hydroxyl
radicals: OH) able to undergo secondary reactions (Figure 4.4).
It is an useful pretreatment for hazardous and non-
biodegradable contaminants to enhance their biodegradability.
Photocatalysis can also be used as a polishing step to treat
recalcitrant organic compounds. The major barrier for its wide
application is the slow kinetics due to limited light fluence and
photocatalytic activity. Si, TiO2, ZnO, WO3, CdS, ZnS, SrTiO3,
SnO2, WSe2, Fe2O3, and so on. can be used as photocatalysts and
Table 4.2 shows band gap energies of those catalysts.
Table 3.2 Bandgap energy of various photocatalysts
Photocatalys Bandgap Photoc Bandgap energy

t energy atalyst (eV)
(eV)
Si 1.1 ZnO 3.2
TiO2 (rutile) 3.0 TiO2 3.2
(anatase
)
WO3 2.7 CdS 2.4
ZnS 3.7 SrTiO3 3.4
SnO2 3.5 WSe2 1.2
Fe2O3 2.2 α– 3.1
Fe2O3
Fig. 3.5 (a) The photocatalytic
oxidation of organic compounds
from textile wastewater under
UV-TiO2 process and (b)
Schematic excitation of
semiconductor by band gap
illumination
3.2.4 Nanomembrane in wastewater treatment
Traditional water treatment methods include physical separation

techniques for particle removal; biological and chemical
treatments to remove suspended solids, organic matter and
dissolved pollutants or toxins; and evaporative techniques and
other physical and mechanical methods. Membrane separation
replaces or supplements these techniques by the use of
selectively permeable barriers, with pores sized to permit the
passage of water molecules, but small enough to retain a wide
range of particulate and dissolved compounds, depending on their
nature. Membrane filtration processes are classified according
to the membrane pore sizes, which dictate the size of the
particles they are able to retain .
Fabrication of MoS2 nanosheet membrane. (A) Schematic process to produce MoS 2 nanosheets from layered bulk
materials in the CO2/ethanol/ water system environment by vacuum filtration method. (B) Preparation of MoS 2
nanosheets by lithium-intercalated MoS2 dispersion and vacuum filtration. (C) Schematic representation of synthesis
of a 2D Ti3C2Tx membrane from Ti3AlC2 and photograph and cross-sectional SEM image of a Ti 3C2Tx membrane.
(D) 2D lamellar MXene membrane nanosheets on AAO support. (E) Freestanding BN-laminated membrane, photo
of the colloidal solution of few-layer BN. Photo of a piece of freestanding BN membrane with size 15 mm 4 mm.
Cross-sectional SEM image of a BN membrane, with the inset showing the lamellar structure of the BN membrane
constructed by few-layer BN sheets and AFM image of fewlayer BN nanosheets on a mica substrate, with the
corresponding height profile (inset) along the blue line showing thicknesses and lateral sizes of the nanosheets
3.2.4 Nanomembrane in wastewater treatment
However, the effectiveness of many membranes can be improved;

for example by enhancing the flux or by reducing membrane
fouling. Membrane characteristics that can be improved by the
use of nanoparticles are: antifouling and antimicrobial properties;
increased selectivity; increased flux (through increased
hydrophobicity); or poresize control by nanogels
(shrinking/growing by change of pH or temperature). The
application of nanoparticles in membranes can thus decrease the
energy demand, the use of chemicals for membrane cleaning, and
cost.
3.2.5 Antimicrobial activity
Microbial contamination of water poses a major threat to public
health. With the emergence of microorganisms resistant to multiple
antimicrobial agents (Barnes et al. 2006) there is increased demand
for improved disinfection methods. Current advances in the field of
nanobiotechnology, the ability to prepare nanomaterials of specific
size and shape, are likely to lead to the development of antibacterial
agents for application in wastewater. Reducing the size of the
materials is an efficient and reliable tool for improving
biocompatibility. However, little is known about how the biological
activity of certain materials changes as the size of the constituting
particles decreases to nanoscale dimensions. The functional activities
of nanoparticles are influenced largely by the particle size.
Antibacterial activity is related to compounds that locally kill bacteria
or slow down their growth, without being in general toxic to
surrounding tissue.
3.2.5 Antimicrobial activity
1. Metal nanomaterials
 Ag Nanoparticles
 Au Nanoparticles
2. Metal oxide nanomaterials

 CuO nanomaterials
 MgO nanomaterials
 TiO2 nanomaterials
 ZnO nanomaterials
 Al2O3 nanomaterials
Wastewaters Treatment Part Ⅱ
Contents

case study)
removal
3.3 Synthesis techniques of
nanomaterials (including case study)
3.3.1 Introduction
The synthesis of nanomaterial can be well accomplished by two broad
approaches (Figure 3.3-1). These two approaches are ‘Top–down’ and
‘Bottom–up’.
Figure 3.3-1 Synthesis route of nanomaterials.

Example ：
NUCLEATION
3.3.2 CHEMICAL SYNTHESIS METHOD OF NANOMATERIALS
3.3.2.1 Chemical precipitation technique
Chemical synthesis has been the predominant method to
developing new materials with novel properties for technological
applications. It is comparatively easy to design materials of
varied morphology and composition with a better control through
a chemical synthesis.
The major difficulty in the chemical precipitation method is to
eliminate the contamination, particularly due to the by-products
generated in the chemical reactions. The optimization procedure is
lengthy.
① Microwave irradiation technique
Compared with conventional methods, microwave synthesis has the
advantages of short reaction time, generating small particle size,
and narrow particle size distribution with high purity. Thus,
microwave irradiation as a heating method has found numerous
applications in synthetic chemistry. Particles of very small sizes
show unique physical properties. With the decrease in particle size,
an extremely high surface to volume ratio is obtained. This leads to
an increase in surface specific active sites for chemical reactions
and photon absorption that enhance the reaction and absorption
efficiency. The enhanced surface area increases surface states,
which changes electron and hole activities and affects the chemical
reaction dynamics.

① Microwave irradiation technique
Figure 3.3-2. Principle of conventional and microwave heating methods.

② Chemical vapor deposition technique
It is a chemical process used to produce high-purity, high-
performance solid materials. The process is often used in the
semiconductor industry to produce thin films. In a typical CVD
process (Figure 3.3-3), the wafer (substrate) is exposed to one or
more volatile precursors, which react and/or decompose on the
substrate surface to produce the desired deposit.

Frequently,
volatile by-
products are
also produced,
which are
removed by
gas flow
through the
reaction
chamber.
Figure 3.3-3 A schematic of a chemical vapor deposition

reactor.
To avoid undesired chemical reactions, the

substrate surface temperature, deposition time,
pressure and type of surface is carefully selected.
③ Vapor-phase synthesis technique
In vapor-phase synthesis of
nanoparticles, the formation of
nanoparticles takes place in gas
phase (Figure 3.3-4). In this
synthesis technique the
condensation of atoms and
molecules is carried out.
Figure 3.3-4 Schematic representation of Vapor-

phase synthesis of single phase nanomaterials.
The vapor phase synthesis is not

new and many multinational
companies have been using flame
reactors (Figure 3.3-5) for
decades for producing large
quantities of nanoparticles. The
flame reactors were used for
forming various nanoparticles
such as carbon black and
titanium dioxide. Figure 3.3-5 Flame assisted synthesis of
nanomaterials.

④ Hydrothermal synthesis technique
Hydrothermal synthesis can be defined as a method of synthesis
of single crystals which depends on the solubility of minerals in
hot water under high pressure. The crystal growth is performed
in an apparatus consisting of a steel pressure vessel called
autoclave (Figure 3.3-6), in which a nutrient is supplied along with
water. A gradient of temperature is maintained at the opposite
ends of the growth chamber so that the hotter end dissolves the
nutrient and the cooler end causes seeds to take additional
growth.

④ Hydrothermal synthesis technique
Figure 3.3-6 Hydrothermal synthesis of nanomaterials (K. Zajaczkowski,

Solvothermal Synthesis, 2011).

④ Hydrothermal & solvothermal synthesis technique
The hydrothermal process is one of the most well-known and extensively
used methods used to produce nanostructure materials. In the hydrothermal
method, nanostructured materials are attained through a heterogeneous
reaction carried out in an aqueous medium at high pressure and the
temperature around the critical point in a sealed vessel.
The solvothermal method is like the hydrothermal method. The only
difference is that it is carried out in a non-aqueous medium. Hydrothermal
and solvothermal methods are generally carried out in closed systems. The
microwave-assisted hydrothermal method has recently received significant
attention for engineering nanomaterials, combining the merits of both
hydrothermal and microwave methods. Hydrothermal and solvothermal
methods are exciting and useful methods for producing various nano-
geometries of materials, such as nanowires,nanorods, nanosheets, and
nanospheres.
⑤ Micro-emulsion technique
This is relatively a new technique,
which allows preparation of ultrafine
metal particles within the size range 5
nm <particle diameter <50 nm. The rate
of particle nucleation is a function of
the percolation degree of micro-
emulsion droplets (Figure 3.3-7).
Besides a short introduction into some
aspects of the micro-emulsion types
and formation, here the kinetics of
metallic particle formation using
micro-emulsion discussed.
Figure 3.3-7 Micro-emulsion technique synthesis of nanomaterials.


Types of Micro-emulsion

⑥ Sonochemical technique
In this technique, nanoparticles are prepared by irradiating the
aqueous or organic dispersion of precursor materials using an
ultrasonic probe at room temperature. The size of the particles
obtained in this method mainly depends on the solution
concentration and the time of sonication. MnO2 nanoparticles,
CdSe nanomaterials, and CeO2 nanparticles have been synthesized
using sonochemical technique.
⑥ Sonochemical technique
3.3.3 Physical synthesis method of Nanomaterials
3.3.3.1 Laser ablation technique
In laser ablation, high-power laser pulses are used to evaporate
matter from a target surface such that the stoichiometry of the
material is preserved in the interaction. As a result, a supersonic jet
of particles (plume) is ejected normal to the target surface. The
plume, similar to the rocket exhaust, expands away from the target
with a strong forward-directed velocity distribution of the different
particles. The ablated species condense on the substrate placed
opposite to the target.
3.3.3.1 Laser ablation technique
3.3.3.2 Sputtering technique
A technique used to deposit thin films of a material onto a

surface (‘substrate’). By first creating gaseous plasma and then
accelerating the ions from this plasma into some source material
(‘target’), the source material is eroded by the arriving ions via
energy transfer and is ejected in the form of neutral particles-
either individual atoms, clusters of atoms or molecules.
3.3.3.2 Sputtering technique
3.3.3.3 Spray route pyrolysis technique
Nanometer-sized particles (1–100 nm) are of considerable interest
for a wide variety of applications, ranging from electronics via
ceramics to catalysts, due to their unique or improved properties that
are primarily determined by size, composition and structure. A simple,
rapid and generalizable aerosol decomposition (spray pyrolysis)
process is used for the continuous synthesis of nanoparticles with
adjustable sizes, narrow size distribution, high crystallinity and good
stoichiometry .
3.3.3.4 Inert Gas Condensation technique

3.3.3.4 Inert Gas Condensation technique
An inert gas condensation technique has been used to

prepare nanometer-sized particles of metallic iron by
evaporation and agglomeration in a flowing inert gas stream.
It is the most advanced technique, although the technique is
costly, it is considered as a controlled process as by this
method the exact shape and size of the nanoparticle can be
synthesized. In inert gas condensation technique, the
nanoparticle as soon as they formed rapidly collides with
inert gas in a low-pressure environment and thus smaller and
controlled nanoparticles are formed (Gracia-Pinilla et al.
2010; Pe´rez-Tijerina et al. 2008).
3.3.4 Case studyⅠ: Synthesis of Ca(OH)2 nanoparticles
3.3.4.1 Introduction
Calcium hydroxide (Ca(OH)2) belongs in the category of moderately
soluble compounds. Literature on the preparation of moderately
water soluble inorganic nanoparticles is rare (Rees et al. 1999),
compared to the studies concerning nanoparticles of water insoluble
compounds. Wilhelmy & Matijevic´, (1984) reported that the
precipitation of metal hydroxide from corresponding salt solution is
affected by reaction time and temperature (Matijevic´ & Scheiner,
1978; Sugimoto & Matijevic, 1980). Particularly, above 100◦C
temperature, formation of nano-scale particles is rapid and sizes are
found to be uniform . Metal hydroxide precipitation is also affected
by concentration of reacting species and type of medium. Hamada &
Matijevic reported that selection of organic solvents can influence
size and shape of the particles obtained by the precipitation
reaction.
3.3.4.2 EXPERIMENTAL DETAILS

①Synthesis of Ca(OH)2 nanoparticles
Ca(OH)2 nanoparticles were synthesized by a wet chemical

method involving dispersion of the metal salt in organic
solvent (ethylene glycol) without using surfactant. In a
typical run, 25 mL of ethylene glycol (EG) was heated in a
conical flask at 150◦C, in an oil bath, for 30 min. 12.09 g of
Ca(NO3)2 4H2O was mixed with the solvent. After dissolving
Ca(NO3)2, 12 mL of NaOH solution (0.7 M) was added
dropwise into this mixture while stirring for 10 minutes at
50 rmp. Ca2+–EG complex thus obtained was aged for 5
minutes at room temperature. After that, the supernatant
was discarded, and powders were collected by hot vacuum
filtration with a 0.45 μm Whatman filter paper.

①Synthesis of Ca(OH)2 nanoparticles
②Characterizations of Ca(OH)2 nanoparticles

The phase analysis and crystal structure of Ca(OH)2 was studied
by X-ray diffractograms (XRD).
Particle sizes and morphology were studied with a field emission
scanning electron microscope (FESEM) of Carl Zeiss model
Supra-40 (with an accelerated voltage 200 kV) and a high-
resolution transmission electron microscope (HRTEM) of JEOL
(JEM-2100), with an operating voltage 200 kV.
The average compositional analysis for Ca(OH)2 were studied
with in situ EDS in conjunction with the FESEM imaging of
selective regions.
The IR spectra of thin pellets of nanoparticles in forms of
powders in a KBr matrix were studied. A NexusTM 870 FT–IR
(Thermo Nicolet, USA) spectrophotometer equipped with a
deuterated triglycine sulfate thermoelectric cool (DTGS-TEC)
detector collected the data over a range 500–4000 cm−1.
3.3.4.3 RESULTS AND DISCUSSION
Nucleation reactions in the homogeneous phase provide several

chemical pathways for obtaining calcium hydroxide nanoparticles. A
better control of particle characteristics seems to be offered by
judicious choice of counterions of the calcium salt solutions.
Counterions of calcium source salts affect the size and the specific
surface area of crystallites with a trend that follows a Hofmeister
series of anions: (sulfate < chloride < nitrate < perchlorate). The size
of particles obtained by the hydrolysis of calcium nitrate in ethylene
glycol/aqueous NaOH solution depended on experimental conditions
such as reaction temperature, aging time, concentration of NaOH, and
concentration of calcium nitrate. Table 1 represents conditions under
which particles of different size were produced.
Table 3.3-1 Experimental conditions on average particle size of

calcium hydroxide nanoparticles.
Synth Reaction solvent Temperatur NaOH((mol Ca(NO3)2 Aging time Average

esis e(◦C) L−1) (mol L−1) (minutes) particle
route size (nm)
1 Ethylene glycol 150 0.70 0.50 40 80–100

2 Ethylene glycol 115 0.70 0.50 40 >180
3 Ethylene glycol 150 0.70 0.50 25 60–80
4 Ethylene glycol 150 0.70 0.50 5 35–65
5 Ethylene glycol 115 0.70 0.50 5 >100
6 Ethylene glycol 150 1.50 0.50 25 >120
7 Ethylene glycol 150 1.50 0.75 40 60–110
8 Ethylene glycol 150 1.50 0.75 5 –
9 Ethylene glycol 115 1.50 0.75 25 –
10 Ethylene glycol 150 0.12 0.10 40 –

①X-ray diffraction of Ca(OH)2 nanoparticles
Figure 3.3-8 The XRD patterns of Ca(OH)2

nanoparticles: (a) immediately after synthesized and
(b) after 45 days
①X-ray diffraction of Ca(OH)2 nanoparticles
As marked by (hkl) values, all the peaks in the diffractograms were
indexed in terms of a hexagonal crystal structure of P3¯m1 space
group. Despite little variation in relative peak intensities in the
diffractograms, the peak positions (interplanar spacing dhkl ) varied due
to the variation in the lattice
Table 2 A comparison in typical structural parameters of synthesized

nanoparticles and bulk Ca(OH)2.
Average Volume Surface

Parameter a c Density(ρ)
Size (D) (V) area
(Å) (Å) (g cm−3)
(nm) (nm3) (m2 g−1)
Bulk 3.596
4.9278 0.05520 2.22 –
Ca(OH)2 6
After 3.595
4.9277 35 0.05514 2.23 56.84
synthesis 6
After 45 3.591
4.9329 46 0.05518 2.22 47.08
days 4

②Microstructure of Ca(OH)2 nanoparticles
Figure 3.3-9 FESEM micrograph of Figure 3.3-10 TEM image of synthesized Ca(OH)2
synthesized Ca(OH)2 nanoparticles with nanoparticles with HRTEM (inset bottom right
inset EDX. corner) and particle diameter histogram (inset top
right corner).
②Microstructure of Ca(OH)2 nanoparticles
Figure 3.3-11 Selected area diffraction (SAD) pattern of synthesized Ca(OH) 2 nanoparticles.

③ FTIR studies of Ca(OH)2 nanoparticles
Figure 3.3-12 FTIR spectra of Ca(OH)2 nanoparticles (a) immediately

after synthesized and (b) after 45 days.
Figure 3.3-12 compares FTIR spectra for Ca(OH)2

nanoparticles (a) immediately after synthesis and (b) aged
after 45 days. In Figure, no peaks were observed for metal
glycolate in the sample (Tekaia- Elhsissen et al. 1989). The
peak at 3642.41 cm−1 is detected due to the O–H stretching of
the solid Ca(OH)2 (Ryskin & Farmer, 1974). A similar FTIR
result was reported by Salvadori & Dei, (2001) in Ca(OH)2
nanoparticles prepared by diol as a solvent. In Figure 3.3-12 ,
peaks of CaCO3 at 876.08 and 1473.34 cm−1 were also
observed due to the partial carbonation of Ca(OH)2 particle
when it was peptized. In comparision with sample (a) and
sample (b) intensity for O–H stretching of solid Ca(OH)2
decreased at 3642.14 cm−1 wavelength, whereas intensity at
876.08 and 1473.34 cm−1 wavelength for CaCO3 increased.
The origin of the high reactivity of Ca(OH)2 nanoparticles towards CO2

resides is greatly dependent on the activity of the large particles
surface. Colloidal Ca(OH)2 particles with greater average size
synthesized in previous studies showed only partial carbonation.
Therefore, the high reactivity of the synthesized particles was
observed and attributed to the very small size of particles that not
only produces a highly active surface area (52 m2g−1), but also does not
allow the formation of a protective CaCO3 layer on the Ca(OH)2
particles surface. From the XRD pattern of 45 days of Ca(OH)2
nanoparticles, no peak for CaCO3 was observed. It indicates that bulk
carbonation did not take place, referring that synthesized Ca(OH)2
nanoparticles are stable up to 45 days in a capped bottle under normal
condition.
Wastewaters Treatment Part Ⅱ
Contents

case study)
removal
3.4 Performance of nanomaterials in
heavy metals removal
This part discusses the experiments required for batch test to
evaluate heavy metals removal efficiency of different nanoparticles
synthesized in last part.
Dissolution properties of synthesized Ca-based nanoparticles were
investigated via successive batch tests. Factors such as time, pH o
f the solvent, and dose effects on dissolution of nanomaterials wer
e studied. In batch studies, different factors and their applicabilit
y were estimated to obtain optimum results. Batch tests involved p
erforming tests to investigate the optimization parameters for tre
atment of heavy metals from synthetic wastewater-focusing prima
rily on pH and time. To evaluate the removal efficiency of synthesi
zed Ca-based nanomaterials with their bulk materials, dose depend
ent batch tests were also performed.
3.4.1.2 Experimental details
① Materials
Synthesized nanoparticles discussed in last part, were used in conducting
the batch tests. Lime and bulk calcium sulfide were procured from a
commercial source. Solutions containing Fe(II), Cu(II), Cd(II), Co(II),
Ni(II), Pb(II), and Zn(II) were synthesized from their respective
standard reagent grade metal sulfate and nitrate salts (Merck,
Germany). Each metal salt, ferrous sulfate heptahydrate (FeSO4 7H2O),
copper sulfate pentahydrate (CuSO4 5H2O), cadmium sulfate octahydrate
(CdSO4 8H2O), cobalt sulfate heptahydrate (CoSO4 7H2O), nickel sulfate
heptahydrate (NiSO4 7H2O), lead nitrate (Pb(NO3)2), and zinc sulfate
heptahydrate (ZnSO4 7H2O), were dissolved in MilliQ water at a
concentration of 100 mg L−1 of each heavy metal, for precipitation studies
and at a concentration of 100 mg L−1 of each heavy metal, for the pH
dependence study. The pH of heavy metals containing solution was
maintained in the range of 1.99–2.02.
② Solubility of Ca-based nanoparticles and commercial lime and
Calcium sulfide
A solubility study of three nanoparticles was conducted in Milli-
Q water without addition of any electrolyte. The effect of dose
on solubility of nanoparticles was carried out by dissolving known
weight (0.1 to 2.0 g L−1) of three Ca-based nanoparticles and
commercial lime and calcium sulfide separately, in 250 mL capped
flasks containing Milli-Q water and agitated with in magnetic
stirrers with 100 rpm at 25◦C for 2 hours. The rate of the
solubility tests of three Ca-based nanoparticles and lime and
calcium sulfide were performed by dissolving a known weight (0.1
g L−1) of three Ca-based nanoparticles and lime in 500 mL capped
flasks containing Milli-Q water and agitated with magnetic
stirrer at 100 rpm at 25◦C for 2 hours.
③ Dose dependent study for heavy metals removal using Ca(OH)2, CaO
nanoparticles and Lime
A dose dependent study was conducted using a known dosage (0.10,
0.25, 0.50, 0.75, 1.00, 1.25, 1.50, 1.75 and 2.00 (± 0.01) g L−1) of
Ca(OH)2, CaO nanoparticles, and commercial lime. In 1000 mL
beakers, 500 mL of synthetic effluent was treated with each dosage
of Ca(OH)2, CaO nanoparticles, and lime separately. Each sample was
mixed at 100 rpm by a jar test apparatus for 30 minutes at room
temperature. After mixing, samples were allowed to settle for 1
hour. The supernatant was sampled without filtration or other
treatment in order to approximate a realistic application. After
measuring the pH of each supernatant, the supernatant was
digested with concentrated HNO3 to determine total heavy metal
concentrations by atomic absorption spectroscopy (AAS–GBC
SensAA). All samples were replicated five times (from the initial
③ Dose dependent study for heavy metals removal using Ca(OH)2, CaO
nanoparticles and Lime
The heavy metals removal capacity of synthesized nanomaterials

was calculated according to following equation:
where C0 and Ct (mg L−1) are initial concentration and the

concentration of heavy metal ions at any time t, respectively.
④ Reaction time dependent study for heavy metals removal using
Ca(OH)2 and CaO nanoparticles
After determining a suitable dosage of Ca-based

nanoparticles in the previous section, similar
experimental methodologies were employed for reaction
times of 5, 10, 15, 30, 45 and 60 minutes. After being
mixed and allowed to settle, the supernatant was
sampled and measured for pH, and then digested with
concentrated HNO3 for determining total heavy metal
concentrations by AAS. All samples were replicated five
times.
⑤ Sludge volume study
The volume of the decanted sludge was estimated by the

volumetric method using Imhoff cones. After 30 minutes
of settling, the volume of sludge produced was
determined by directly the mL L−1 of wastewater
treated. The solids were then filtered, dried at 105◦C
for 24 hours, and weighed. Solid precipitates were
characterized by X-ray diffraction analysis.
⑥ Leaching study
To evaluate the likely performance of precipitates in a

landfill environment, the precipitate sludge was tested for
its leachabilites following the procedure DIN38414–S4
(Din-Normen, 1984). The vacuum oven dried sludge of 10 g
(crushed to <10 mm) was rotated on a roller at 30 rpm with
100 mL of distilled water for 24 hours at an ambient
temperature of 25 1◦C. The solid/liquid ratio was 1:10. The
vessels were centrifuged and the supernatant liquids
filtered through a 0.45 μm membrane filter prior to
acidification and analysis by AAS. Leaching experiments
were performed in duplicate and all analyses were
conducted in triplicate, and reported as an average of the
values obtained.
⑦ Dose dependent study for heavy metals removal using CaS
nanoparticles and bulk Calcium sulfide
A dose dependent study was conducted using known dosages
(0.10, 0.25, 0.50, 0.75, 1.00, 1.25, 1.50, 1.75 and 2.00 (± 0.01) g
L−1) of CaS nanoparticles and calcium sulfide. In 1000 mL
beakers, 500 mL of synthetic effluents were allowed to react
with each dosage of CaS nanoparticles and bulk calcium sulfide
separately. Each sample was mixed at 100 rpm in a jar test
apparatus for 30 minutes at room temperature. After mixing,
the samples were allowed to settle for 1 hour. The supernatant
was sampled without filtration or other treatment in order to
approximate a realistic application. After measuring the pH of
each supernatant, the supernatant was digested with
concentrated HNO3 for determining total heavy metal
concentrations by AAS. All samples were replicated five times
(from the initial stage).
⑧ pH dependent study for sulfide precipitation using CaS nanoparticles
After determining a suitable dosage of CaS

nanoparticles in the previous section, similar
experimental methodologies were employed for the pH
dependent study with different pH conditions of
synthetic wastewater (2.5, 3.5, 4.5, 5.5, 6.0, 6.5, 7.0,
8.5, and 9.5). After being mixed and allowed to settle,
the supernatant was then digested with concentrated
HNO3 for determining total heavy metal
concentrations by AAS. All samples were replicated
five times.
3.4.1.3 Results and discussion
① Solubility of Ca-based nanoparticles
Figure3.4-1 Effect of time (a), effect of pH (b), and effect of doses (c)
on solubility of Ca-based nanoparticles and lime (Dose 0.25 g L−1, pH 7.0 for
120 minutes).

② Heavy metal removal
Chemical precipitation is widely used for heavy metal

removal from inorganic effluents. After the pH is adjusted
to the basic condition, the dissolved metal ions are
converted to the insoluble solid phase via a chemical reaction
with a precipitating agent. Usually, the precipitates will
remain suspended in the water. Therefore, the removal
effect may not be satisfactory. In this work, Ca-based
nanoparticles and commercial lime were separately added in
an incremental way to remove metal ions, until it leveled off
at 97.72%– 99.84%.
③ Dose dependent study for heavy metals removal using Ca(OH) 2 and
CaO nanoparticles
The removal of heavy metals from synthetic effluent was
investigated using Ca(OH)2 and CaO nanoparticles and lime at nine
dosage levels (0.10, 0.25, 0.50, 0.75, 1.00, 1.25, 1.50, 1.75 and
2.00 (± 0.01) g L−1). As nanoparticle dosages were increased, the
temperature rose slightly (around 0.2–0.6◦C), due to the various
complex minerals contained in the synthetic effluents. Tables 3
and 4 indicate that increasing the dosage of Ca-based
nanoparticles caused a rise in pH in the tested effluents. It is
clear that the removal of heavy metals gradually increased with
increasing pH, until reaching the equilibrium.
CaO nanoparticles
This effect suggests that Ca-based nanoparticles could be used to
raise the solution pH in order to lower the solubility of the
metallic constituent, and thus to bring about precipitation.
Precipitation with Ca(OH)2 and CaO nanoparticles would constitute
various hydroxides. Metal carbonates could also be generated
since the reactions of carbonate ions in aqueous solution are the
following:
CaO nanoparticles
Table 3 Heavy metal removal and final pH of solution after treatment with
different dosages of Ca(OH)2 nanoparticles.
aC0 is initial concentration of heavy metal bCf is final concentration of heavy metal cC0 is initial
concentration of heavy metal dCf is final concentration of heavy metal eC0 is initial concentration of
heavy metal fCf is final concentration of heavy metal gC0 is initial concentration of heavy metal hCf is
final concentration of heavy metal iC0 is initial concentration of heavy metal jCf is final concentration
of heavy metal kC0 is initial concentration of heavy metal lCf is final concentration of heavy metal mC0 is
initial concentration of heavy metal nCf is final concentration of heavy metal
CaO nanoparticles
Table 4 Heavy metal removal and final pH of solution after treatment
with different dosages of CaO nanoparticles.
aC0 is initial concentration of heavy metal bCf is final concentration of heavy metal cC0 is initial
concentration of heavy metal dCf is final concentration of heavy metal eC0 is initial concentration of
heavy metal fCf is final concentration of heavy metal gC0 is initial concentration of heavy metal hCf is
final concentration of heavy metal iC0 is initial concentration of heavy metal jCf is final concentration
of heavy metal kC0 is initial concentration of heavy metal lCf is final concentration of heavy metal mC0
is initial concentration of heavy metal nCf is final concentration of heavy metal
CaO nanoparticles
Figure 3.4-2 Ca(OH)2 nanoparticles dose

dependent heavy metal removal.
CaO nanoparticles
Figure 3.4-3 CaO nanoparticles dose dependent heavy metal removal.

④ The role of pH on surface charge
The following general equations show the effect of pH on the
surface charge of metal oxides and hydroxides
Thus, the H+ ion acts as a potential determining ion and

effects surface charge. The minimal solubility of the
hydroxides of the majority of metals is reached at an
approximate pH of 9.5–10.0.

⑤ Reaction time dependent study for heavy metals removal
The removal of heavy metals from synthetic effluent using the two
selected dosages for two nanoparticles (1.5 and 2.0 g·L−1 for
Ca(OH)2 and 1.75 and 2.0 g·L−1 for CaO) were examined at six
different reaction times (5, 10, 15, 30, 45 and 60 minutes) (Figures
3.4-4 and 3.4-5).
Figure3.4-4 The removal efficiency for heavy metals after treatment with 1.5
(a) and 2 (b) g L−1 of Ca(OH)2 nanoparticles at different reaction times.

Figure3.4-5 The removal efficiency for heavy metals after treatment with 1.75
(a) and 2 (b) g·L−1 of CaO nanoparticles at different reaction times.

The results reveal that, by increasing the reaction time between the
synthetic effluent and the Ca(OH)2 or CaO, an increase in the removal
efficiency of most heavy metals occurs until equilibrium is reached. It
is clear from the results that the reaction time required for the
maximum removal of Fe(II), Cu(II), Pb(II), Cd(II), Ni(II), Co(II), and
Zn(II) treated with both selected dosages of CaO was approximately
15 minutes. For Ca(OH)2, the optimal reaction times for maximum
removal were 15 minutes for all heavy metals, for both 1.5 and 2.0 g
L−1 dosages. The results for Pb(II), however, differed for the
dosages. According to these results, a large number of heavy metals
were removed when the equilibrium reaction time was at 15 minutes.
This time length permitted the settling of these wastes, producing a
clear supernatant. A 15 minutes reaction time was therefore selected
for further study.

⑥ Selected treatment conditions study for heavy metals concentration
From the previous studies described in Section 3.4.1.2③, the
selected dosages of Ca(OH)2 nanoparticles were 1.5 and 2.0 g·L−1
and CaO nanoparticles were 1.75 and 2.0 g·L −1, and the
selected reaction time (from Section 3.4.1.2④) was 15 minutes.
Four conditions were thus chosen for use in the next stages of
the research (Table 4).
Table 4 The results of heavy metals concentration after treatment at selected conditions .

⑦ Selected treatment conditions study for heavy metals removal
Under all four treatment conditions, the residual concentrations of

Pb(II) did not meet the EPA effluent standard (CFR, 40) (0.1 mg·L−1).
The minimum Pb(II) concentration was found when using 1.5 g·L−1 of
Ca(OH)2 nanoparticles and 1.75 g·L−1 of CaO nanoparticles. For Cu(II),
using 1.5 and 1.75 g·L−1 of Ca(OH)2 nanoparticles and CaO nanoparticles
respectively gave a residual concentration which met the effluent
standard limit (2.0 mg·L−1). Zn(II), following all selected treatment
conditions, had a residual concentration which met its effluent
standard limit (5.0 mg·L−1); the minimum concentration was obtained
when using 1.5 and 1.75 g·L−1 of Ca(OH)2 and CaO nanoparticles,
respectively.

⑧ Sludge volume study
Table 4 shows the sludge volume for all selected treatment conditions.
It was found that the final sludge volume depended on the dosage used
to precipitate heavy metals. As is shown in Table 4, treatment by CaO
nanoparticles resulted in lower sludge production. The amount
recorded was 68–88 mL·L−1 for CaO nanoparticles (depending on the
dosage), compared to 72–100 mL·L−1 for Ca(OH)2 nanoparticles, showing
that with CaO nanoparticles, the treated wastewater could be more
easily filtered. This phenomenon may be attributed to the destructive
adsorption effect of CaO nanoparticles (Wagner et al. 2000; Oladoja
et al. 2011).

⑨Precipitate characterization (XRD)
Precipitates were collected and characterized by XRD. The XRD

spectrum (Figure 3.4-6a and 3.4-6b) of precipitates shows heavy
metals were precipitated as metal hydroxide, and sulfate was removed
by precipitation of gypsum (Ca(SO4)2). XRD spectrum in Figure 3.4-6a
shows a large amount of metals was precipitated along with sulfate
(SO2−) that was absent in the Figure 3.4-6b. CaO nanoparticles remove
heavy metals but it seems to have less ability to remove sulfate from
the sample wastewater.

⑨Precipitate characterization (XRD)
(a) (b)
Figure 3.4-6 The XRD spectrum of precipitate (a) treated with Ca(OH) 2
nanoparticles and (b) treated with CaO nanoparticles.

⑩ Leaching study
Though treatment with Ca-based nanoparticles generates a small
amount of sludge, the leaching capacity of heavy metals from the
sludge/sediment under specific treatment condition was evaluated.
The results obtained from the leaching of sludge are also
presented in Table 5. Without any pre-treatment sludge/sediment
was tested for leaching.

⑩ Leaching study
Table 5 shows at different conditions small amounts of heavy
metals were leached from the sediment or sludge. The heavy
metals of interest in the leaching solution were Fe(II), Cu(II),
Cd(II), Pb(II), Ni(II), Co(II), and Zn(II). However, of those
methods, only Cd(II) and Pb(II) are regulated under the EPA
limits.
Comparing the results with the regulatory criteria, it was found
that the leaching of heavy metals from nanoparticle generated
sludge/sediment were lower than the regulatory limits. It also can
be seen that the release of heavy metals from the CaO
nanoparticles precipitates was much lower than that from the
Ca(OH)2 nanoparticle precipitates. From the leaching study, one
can conclude that the generated sludge/ sediment from all
selected treatment conditions is fit for inert waste landfill site
with relative safety, especially in relation to the contamination of
the groundwater.

⑾ Dose dependent study for heavy metals removal using CaS
nanoparticles
The removal of heavy metals from synthetic effluent was
investigated using Ca(OH)2 and CaO nanoparticles and lime at nine
dosage levels (0.1, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8 and 2.0
( 0.01) g L−1).
Figure 3.4-7 Bulk CaS dose dependent Figure 3.4-8 CaS nanoparticles dose
heavy metal removals. dependent heavy metal removals.

⑾ Dose dependent study for heavy metals removal using CaS
nanoparticles
From Figure 3.4-7, it is observed that as the bulk CaS

dose increased, the heavy metals removal efficiency also
increased. For the case of Cu(II), the removal efficiency
reached a maximum of 99.95% using a dose of 1.8 g·L−1.
Comparing the test results it is observed that higher

heavy metal removal capability of CaS nanoparticles is
achievable and to reach maximum removal of heavy metal
requires doses higher than that using bulk CaS.

⑿ pH dependent study for heavy metals removal using CaS nanoparticles
To study the effect of pH on heavy metals removal from

synthetic wastewater using CaS nanoparticles, a pH
dependent study was performed using a CaS nanoparticles
dose of 1.0 g·L−1 for various pH conditions. The
thermodynamic equilibria involved in metal sulfide
precipitation can be expressed as:

The concentration of sulfur species is a strong function of pH, as

shown in Figure 7.9. The pK2 value in equation 2 is currently the most
reliable value, as measured by Migdisov et al. (2002). From Figure 7.9,
it is observed that above pH 7.0, HS− species predominant in the
aqueous environment.
At pH 7.0, the bisulfide ion and

aqueous H2S, in solution, are in
equal proportions. At pH 7.0 and
above, it is suitable for metal
sulfide precipitation.
Figure 3.4-9 The pH dependence of sulphide

speciation using MINTEQA2 software.

Figure 3.4-10 shows concentration ratio of [C]/[C0] different heavy
metals at different pH conditions. From Figure 3.4-10, it is observed
that as the pH increased, heavy metals removal efficiency also
increased.
It was observed that to treat

heavy metals using CaS
nanoparticles, the pH should
be in the range of 7.0–8.0
from mixed heavy metals-
containing wastewater.
Figure 3.4-10 The pH dependent heavy

metal removal from synthetic wastewater
using CaS nanoparticles.
3.4.1.4 Nanomaterial in the future in wastewater
The nanomaterials most extensively investigated include metal oxide NPs,

including TiO2 and ZnO; CNTs; and nanocomposites. A detailed discussion
of their application in wastewater and water treatment was also provided.
Given the speed at which they are being developed and applied,
nanomaterials have significant potential for treating water and
wastewater.
Further research is needed to address the challenges posed by
nanomaterials. The commercial use of nanomaterials has been limited to a
few types. Future research should focus on improving nanomaterials’
economic efficiency. The possibility of toxicity of nanomaterials to the
environment and human health is also growing with the widespread and
frequent use of nanomaterials in water and sewage systems. There is
evidence that various nanomaterials have potentially harmful health
effects and adverse effects on the environment. However, current
guidelines for determining nanomaterial hazards are inadequate and weak.
To ensure their practical use, nanomaterials must be evaluated
comprehensively for their toxicity.
Class Assignment
• Reading the book Page 125 ： removal of Pb2+ from

water using silica nano spheres Synthesized on
CaCO3 as a Template: Adsorption Kinetics
• Finishing a report about Removal of Pb2+ from water

using nano-CaCO3

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Novel Technology for

 3.1 Introduction to nanotechnology

In 1959, Physics Nobel Laureate Richard Feynman gave a talk at

Nanoscale materials are defined as a set of substances where at

Materials in the nanometer

Nanoscience is similar to materials science in that it is an integrated

The Egyptians used ink containing

Nanoparticles of lead sulfide were

Nanoparticles of gold and silver have

 The first mention of nanotechnology (not yet using that

There are several ways to classify nanomaterials. This depends very

(1) Carbon Based Materials

Figure 3.2 Classification of materials according to the dimensionality of the nanostructures.

Since water treatment by using nanoparticles has potential for

Fig. 3.3 Application of nanotechnology in wastewater treatment.

Fig. 3.4 Common applications of metal

Fig. 3.5 Five types of metal

Nanoparticles formed by metal or metal oxides are another type of

Recently, there have been several reports on magnetic oxides,

Photo-catalyst activated by UV lights can oxidize organic

Figure 3.4 Schematic diagram of photocatalysis.

Table 3.2 Bandgap energy of various photocatalysts

Photocatalys Bandgap Photoc Bandgap energy

Traditional water treatment methods include physical separation

However, the effectiveness of many membranes can be improved;

2. Metal oxide nanomaterials

 3.1 Introduction to nanotechnology

Figure 3.3-1 Synthesis route of nanomaterials.

3.3.2.1 Chemical precipitation technique

Figure 3.3-2. Principle of conventional and microwave heating methods.

3.3.2.1 Chemical precipitation technique

Figure 3.3-3 A schematic of a chemical vapor deposition

② Chemical vapor deposition technique

To avoid undesired chemical reactions, the

Figure 3.3-4 Schematic representation of Vapor-

③ Vapor-phase synthesis technique

The vapor phase synthesis is not

③ Vapor-phase synthesis technique

3.3.2.1 Chemical precipitation technique

Figure 3.3-6 Hydrothermal synthesis of nanomaterials (K. Zajaczkowski,

3.3.2.1 Chemical precipitation technique

3.3.2.1 Chemical precipitation technique

Figure 3.3-7 Micro-emulsion technique synthesis of nanomaterials.

3.3.2.1 Chemical precipitation technique

3.3.2.1 Chemical precipitation technique

A technique used to deposit thin films of a material onto a

3.3.3.4 Inert Gas Condensation technique

3.3.3.4 Inert Gas Condensation technique

An inert gas condensation technique has been used to

3.3.4.2 EXPERIMENTAL DETAILS

Ca(OH)2 nanoparticles were synthesized by a wet chemical

3.3.4.2 EXPERIMENTAL DETAILS

②Characterizations of Ca(OH)2 nanoparticles

3.3.4.3 RESULTS AND DISCUSSION

Nucleation reactions in the homogeneous phase provide several

3.3.4.3 RESULTS AND DISCUSSION

Table 3.3-1 Experimental conditions on average particle size of

Synth Reaction solvent Temperatur NaOH((mol Ca(NO3)2 Aging time Average

1 Ethylene glycol 150 0.70 0.50 40 80–100

3.3.4.3 RESULTS AND DISCUSSION