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Chapter 1
INTRODUCTION TO PERVAPORATION
1.1 BACKGROUND:
Most industrial scale separation processes are based on energy intensive methods
such as distillation, evaporation, and freeze crystallization. Membrane separations offer
significant advantages over existing separation processes. Current membrane separation
technologies can offer energy savings, low-cost modular construction, high selectivity of
separated materials, and processing of temperature- sensitive products [1-5]. Membranes
separate mixtures by discriminating the components on the basis of physical or chemical
attributes, such as molecular size, charge, or solubility [6]. By passing water and
retaining salts, membranes are used to produce over half of the world's desalinized
potable water. Membranes can also separate oxygen and nitrogen from air as well as
hazardous organics from contaminated water in applications such as groundwater
remediation. The need for membrane separation technology increases as environmental
requirements tighten, water circuits close, the recycling of wastes increases and the purity
requirements for foodstuff and pharmaceuticals increase Six major membrane processes
(microfiltration, ultrafiltration, reverse osmosis, electrodialysis, gas separation and
pervaporation) have found use in such application areas as water purification, chemical
and food processing, drug delivery, bioseparations, and medical treatment [1-6].
Compared with traditional separation processes, such as distillation, extraction and
filtration, membrane technology is a relatively new method that has been developed in
the past few decades, but it has been widely adopted in many industries. The membrane
processes have the following distinguishing characteristics [Mulder 1991]:
1) Continuity and simplicity of the processes,
2) Adjustability of the separation properties,
3) Feasibility of incorporation into hybrid processes,
4) Low energy consumption and moderate operating conditions.
Developments in membrane formation techniques and materials
science accelerate the research and applications of membrane
technology. Now commercial membrane applications have successfully
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Separation of Binary Mixture By Using Pervaporation
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among membrane separations, involving the liquid-vapor phase change to achieve the
separation [7, 8].
In Pervaporation (PV), components of a volatile liquid feed will permeate through a
nonporous permselective membrane and evaporate into the permeate space (Figure
1.2.1). The feed components undergo a phase change, making PV a unique membrane
processes (Néel, 1991; Villaluenga and Tabe-Mohammadi, 2000).
Liquid feed flows along one side of the membrane and various feed components
selectively permeate into and through the membrane. In laboratory-scale batch-PV, liquid
retentate is returned to the feed tank, depleted in preferentially permeating components.
The enriched permeate vapour is swept from the membranes downstream surface under
vacuum conditions or by an inert sweep gas, and is collected in a condenser (Feng and
Huang, 1997; Schleiffelder and Claudia, 2001).
Pervaporation, in its simplest form, is an energy efficient combination of
membrane permeation and evaporation. Liquid mixtures can be separated by partial
vaporization through a non-porus permselective membrane. This technique, which was
originally called “Liquid permeation” has subsequently been termed “pervaporation” in
order to emphasized the fact that permeate undergoes a phase change, from liquid to
vapor, during the transport through the barrier.
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Pervaporation can used for breaking azeotropes, dehydration of solvents and other
volatile organics, organic/organic separations such as ethanol or methanol removal, and
wastewater purification.
1.2.2 Possible modes of Pervaporation
Pervaporation units can operate either in the straight-forward or batch mode (Fig.
1.2.3). The straightforward mode is best applied to continuous feed streams, a relatively
small amount of the component to be removed and systems for which concentration
polarization is not a major problem (Fig. 1.2.3(A)). For small streams with large amounts
of one component to separate, or with many different operating conditions, it may be
advantageous to design a batch plant (Fig. 1.2.3(B)) with one or several modules, and a
large feed circulation rate. The product is recycled to the feed tank until the required
concentration is reached. This process simplifies plant design and offers maximum
flexibility, however, with increased utility requirements.
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the difference in partial pressures across the membrane. By reducing the pressure on the
permeate side of the membrane, a driving force is created. Another method of inducing a
partial pressure gradient is to sweep an inert gas over the permeate side of the membrane.
1.2.5Alternative techniques
The requirements for technological or economic operation of the most common
processing techniques for separating organic-organic mixtures are given in Table 2:01.
Separating close boiling organic-organic solvent mixtures by distillation or liquid-liquid
extraction is difficult, as the components have very similar physical and chemical
properties (Young, 1973).
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Work on membrane separations began in the early 1960s, using membrane materials
such as dense metals, zeolites, polymers, ceramics and biological materials. Of these,
polymers are the most widely used material (Smitha et al., 2004). Several different
polymer membrane structures are commonly used today, including porous, dense and
asymmetric membranes. Selecting a good membrane requires a sound knowledge of
membrane structures. Much of the following discussion is based on the excellent review
by Smitha et al. (2004).
1.3.1 Membrane
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recover organics from solutions. These membranes are typically made up of elastomeric
materials (polymers with glass transition temperatures below room temperature). The
flexible nature of these polymers makes them ideal for allowing organic to pass through.
Examples include nitrile, butadiene rubber, and styrene butadiene rubber.
Synthetic membranes are thin, solid-phase barriers that allow preferential passage
of certain substances under the influence of a driving force. Both the chemical and the
physical nature of the membrane material control membrane separation. Membrane
separation occurs because of differences in size, shape, chemical properties, or electrical
charge of the substances to be separated. Microporous membranes control separation by
size, shape and charge discrimination, whereas nonporous membranes depend on sorption
and diffusion. The performance of the membrane is determined by the degree of
separation of fluid mixtures and permeation rate (flux). (3, 33) Three general categories of
inorganic membranes are ceramics, metals and glass. Because they are so rigid, ceramic
microfilters accommodate fluxes five to ten times greater than those of asymmetric
polymeric membranes. They can be backwashed frequently without damaging the
membrane skin layer. Ceramic membranes are highly resistant to cleaning chemicals and
can be sterilized repeatedly by high pressurized steam. Their life span is up to ten years
compared to the typical life spans for polymer membranes, which are about one year for
hydrophobic membranes and up to four years for fluoropolymers. Ceramic membranes
are brittle and are more expensive than polymeric membranes. (3,34) Pervaporation
membranes are typically composites. The first layer is a porous, polymeric support coated
with a second polymer, the "active" or "permselective" layer, which is engineered to
preferentially absorb the chemical species of interest. The membranes’ separation
characteristics can be further refined by varying the thickness of the permselective layer.
(4,88)
For example, asymmetric composite hydrophilic membranes such as composite PVA-
PS (Poly(vinyl alcohol)-Polysulfone) are used for pervaporation. Pervaporation
separation plants contain between ten and one hundred m2 of membrane area, which must
be packaged efficiently and economically into units called membrane modules. Flat-sheet
and spiral-wound modules are commonly used.(3,41) Silicon rubber membranes are also
used in pervaporation. Spiral wound configuration offers a high membrane surface area
per module and allows for relatively high feed flow rates which are common for
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Composite membranes consist of a porous support layer with a thin dense skin
layer on top (Figure 1.4.1 c). The skin is usually a different polymer material from the
support layer. Composite membrane structures minimize membrane cost by reducing the
quantity of expensive high-performance material used. In principle, composite
membranes allow the properties of the dense separating layer and the porous support
layer to be optimized individually, and to a greater extent, than in the phase inversion
process.
1.3.3 Membrane module
When a highly selective material is selected, membrane performance can be
optimized further by reducing the effective membrane thickness. It is best to use a thin
film of the discriminating layer deposited on a highly porous support structure. This
means that either asymmetric or composite membranes have to be developed with a
dense toplayer and an open porous sublayer. The requirements for the sublayer are such
that the resistance for permeate transport must be neglectable compared to the resistance
of the toplayer. Therefore, optimization of the sublayer is very important [12]. It might
even be worthwhile to develop a three layer membrane consisting of a very porous
sublayer, than a nonselective intermediate layer and dense toplayer (Fig. 1.4.3) [12].
The composite membranes can be produced either in a flat configuration or in a
tubular configuration. Membranes have to be incorporated into modules in order to be
used in the process. The main module designs are the plate-and-frame system and the
spiral-wound system that are based on the flat membranes and the tubular, capillary and
hollow fiber modules that are based on the tubular membrane configuration [39]. Fig.
1.4.2 shows a schema of the plate-and-frame module. Plates made of stainless steel form
the feed channels and compartments, which are sealed to the membranes by gaskets. The
membranes are supported by stainless steel perforated plates and spacers, which form the
permeate channels. The latter ones are open to all sides, allowing for a fast and easy
removal of the permeate. The arrangement assures a uniform, parallel flow of the feed
mixture over all membranes in a module.
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The spiral wound modules (Fig. 1.4.3) are flat sheets arranged in parallel to form
a narrow slit for fluid flow. In a typical construction two flat membrane sheets are placed
together with active sides facing the feed spacer.
Membranes are separated by the permeate spacer and glued together on 3 sides.
The fourth side is open and fixed around a perforated centre tube. The feed spacer is
placed outside the membrane and forms the feed channel. The whole assembly is roled
around the centre tube in a spiral and fitted inside the appropriate housing. Such
configuration is compact and relatively inexpensive. Spiral wound modules are used
mainly for organic extraction, with low organic concentration and lower temperatures.
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Chapter 2
LITERATURE SURVEY
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separation mechanisms for different membrane processes [Moon 2000; Matsuura 1994;
Mulder 1991]. Mass transport in non-porous membranes is complicated, but gas
separation and pervaporation share many characteristics.
Electrical potential
Electro dialysis Liquid / Liquid Counter-ion transport
gradient
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Figure 2:1 Schematic diagram of the solution-diffusion model (Lipnizki et al., 1999).
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Figure 2.2 Polymer membrane under liquid permeation conditions with a solution phase
zone and vapour phase zone (Binning et al., 1961).
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which govern selectivity and permeation rate (Qariouh et al., 1999; Villaluenga and
Tabe-Mohammadi, 2000).
2.2.1(B) Selectivity
where xp,i and xp,j are mole fractions of the preferential and secondary permeants
respectively in the permeate, and xf,i and xf,j are the corresponding mole fractions in the
feed. Selectivity can vary from unity (no selective permeation) to infinity, and is affected
by membrane/component solubility, feed hydrodynamic conditions, permeate resistance
due to elevated partial pressures, and changes in diffusion rate due to membrane swelling
(Smitha et al., 2004). Membrane selectivity (especially in organic/organic separations
with components of comparable size) is mainly governed by αS due to the chemical
interaction between permeant molecules and the membrane. Therefore, choosing a
membrane with appropriate affinity is a crucial factor in PV (Villaluenga and Tabe-
Mohammadi, 2000).
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Component permeate fluxes are commonly obtained using the mass transfer
resistance-inseries model (Karlsson and Trägårdh, 1993a; Feng and Huang, 1997).
Overall permeate flux (Jk) for component k, where k = i or k = j for a binary feed is
defined by:
Jk = Cf, k −Hk Cp, k
Rov, k ---------------------- (2.3)
where Cf,k and Cp,k are component feed and permeate concentrations, Hk is a
dimensionless equilibrium partition coefficient (i.e. Ck liq/Ck vap) and Rov,k is the
overall component mass transfer resistance (Smitha et al., 2004)
The pore-flow model for pervaporation was first proposed by Sourirajan et al.
[Matsuura 1994], and Okada et al. [1991] used this model to interpret experimental
observations in pervaporation. In the pore-flow model, it is assumed that there are a
bundle of straight cylindrical pores of specific lengths penetrating across the active
surface layer of the membrane, and all pores are in an isothermal condition [Matsuura
1994]. The mass transport involves
1) Liquid transport from the pore inlet to the liquid-vapor phase boundary,
2) Evaporation at the phase boundary,
3) Vapor transport from the phase boundary to the pore outlet.
The main difference between the solution-diffusion model and the pore-flow
model is the phase change location in the membrane. In the pore-flow model, as shown in
Figure 2.2, the phase change occurs at a certain distance from the membrane surface
contacting with the liquid feed, and accordingly the transport mechanism changes from
liquid permeation to vapor permeation at the liquid-vapor boundary [Matsuura 1994].
Pore-flow model
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The pore-flow model is on the basis of the presence of pores in the membranes, so
whether the pores really exist or how small the pore size is remains hard to answer.
Nonetheless, the theoretical calculations based on the pore flow model have been shown
to be able to reproduce semi-empirical features of the experimental results [Matsuura
1994].
The basic idea of the carrier transport mechanism for pervaporation comes from
biological membranes consisting of polypeptides, and is based on the similarity of the
molecular interactions between the peptides and the functional groups in synthetic
polymers [Moon 2000]. Membranes with carriers are classified into two categories
[Shimidzu and Yoshikawa 1991]: Non-fixed carrier membrane (Liquid membrane) and
fixed carrier membrane. Figure 2.3 shows the mass transport in non-fixed carrier
membranes and fixed carrier membranes. The transport energy in the fixed carrier
membranes is much higher than that in the non-fixed carrier membranes, since adsorption
and desorption are repeated continuously when a permeating component forms a complex
with a carrier in the membrane. On the other hand, once a component forms a complex
with a carrier in a non-fixed carrier membrane, the other component can move only after
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one carrier is released from the former complex formed previously, for which high
selectivity is achieved.
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low selectivities for polar/non-polar organic mixtures, primarily because they did
not have any functional groups to create differential interactions between the
components being separated (Smitha et al., 2004).
2.3.4 Isomers
Mulder et al. (1982) used thin membranes of cellulose esters treated with an
organic solvent to separate isomeric xylenes. Relatively good fluxes but low
selectivities were achieved Since the 1980s a variety of membranes have been used
to extract isomeric components such as xylene isomers, and 1º, 2º or 3º alkanes and
alcohols (Funke et al., 1997; Gump et al., 1999; Wegner et al., 1999; Chen et al.,
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2000; Gump et al., 2000; Nair et al., 2001; Schleiffelder and Claudia, 2001). The
use of PVA membranes for purifying mixed xylenes on an industrial scale has been
limited by the very small separation factors (Smitha et al., 2004).
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as thin as 10-35 μm (Smitha et al., 2004), and modern literature makes little
mention of membrane thickness affecting selectivity.
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YA YA
α => α=
YB
=
(1 − YA)
Separation factor -------------------------------
YA XA
XB (1 − XA)
(01)
YA
Enrichment factor => β β= ---------------------------------------------------
XA
(02)
Where:
XA - weight fraction of preferentially permeating species in the feed phase,
YA - weight fraction of preferentially permeating species in the permeate phase,
with XA + XΒ = 1 and YΑ + YΒ = 1.
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Selecting membrane materials for PV is often done by trial and error. This is
time consuming and the best membrane may not be found due to the limited
number of membranes tested. A more rational method would match the physico-
chemical properties of the membrane material with the components of the liquid to
be separated. This is done simplistically for common PV applications such as
organic liquid dehydration or waste-water treatment by choosing hydrophilic or
hydrophobic membranes. However, hydrophobicity is not a major distinguishing
factor for components in an organic/organic mixtures so a more comprehensive
approach is required.
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The composition and morphology of the membranes are a key to effective use
of membrane technology. The choice of the membrane strongly depends on the type
of application [12]. It is important which of the component should be separated
from the mixture and whether this component is water or an organic liquid.
Generally, the component with the smallest weight fraction in the mixture should
preferentially be transported across the membrane. Looking at the mixtures to be
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Separation of Binary Mixture By Using Pervaporation
separated and their compositions, the following different kinds of pervaporation and
vapor permeation processes can be distinguished [12-23]
For the mixture of two organic liquids or vapors, again three kinds of
mixtures can be distinguished: polar/apolar, polar/polar and polar/apolar mixture.
For the removal of the polar component from polar/ apolar mixture polymers with
polar groups should be chosen and for the removal of the apolar component
completely apolar polymers are favorable. The polar/polar and apolar/apolar
mixtures are very difficult to separate, especially when the two components have
similar molecular sizes. In principle all kinds of polymers can be used for these
systems, the separation has to take place on the basis of differences in molecular
size and shape, since no specific interaction of one of the two components can take
place. Recently, ceramic membranes and membranes pre pared from conducting
polymers have also been used as the selective barriers in pervaporation [24-27].
Ceramic membranes combine high thermal and chemical stability with very high
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However, for separation of organic liquids, the criteria for selecting proper
polymer materials are not very clear yet. Both rubbery polymers and glassy
polymers have been used in research.
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In accordance with the present invention, it has been found that the
pervaporation for separation of binary mixture is good and cost effective by other
method in accordance with the present invention ethanol water mixture is selected
as binary organic mixture and polyvinyl(alcohol) material membrane for the
process.
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Chapter 3
Ethanol, also called ethyl alcohol, pure alcohol, grain alcohol, or drinking
alcohol, is a volatile, flammable, colorless liquid. It is a psychoactive drug, best
known as the type of alcohol found in alcoholic beverages and in modern
thermometers. Ethanol is one of the oldest recreational drugs known to man. In
common usage, it is often referred to simply as alcohol or spirits.
Ethanol, C2H5OH, (also called Ethyl Alcohol) is the second member of the
aliphatic alcohol series. It is a clear colorless liquid with a pleasant smell. Except
for alcoholic beverages, nearly all the ethanol used industrially is a mixture of 95%
ethanol and 5% water, which is known simply as 95% alcohol. Although pure ethyl
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Other names: Ethyl alcohol; grain alcohol; pure alcohol; hydroxyethane; drinking
alcohol; ethyl hydrate.
Ethanol is a versatile solvent, miscible with water and with many organic
solvents, including acetic acid, acetone, benzene, carbon tetrachloride, chloroform,
diethyl ether, ethylene glycol, glycerol, nitromethane, pyridine, and toluene.[9][10] It
is also miscible with light aliphatic hydrocarbons, such as pentane and hexane, and
with aliphatic chlorides such as trichloroethane and tetrachloroethylene.[10]
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miscibility gap tends to get wider with higher alkanes and the temperature for
complete miscibility increases.
Ethanol-water mixtures have less volume than the sum of their individual
components at the given fractions. Mixing equal volumes of ethanol and water
results in only 1.92 volumes of mixture.[9][13] Mixing ethanol and water is
exothermic. At 298 K up to approx. 777 J/mol[14] are set free.
Mixtures of ethanol and water form an azeotrope at approx. 89 mole-% ethanol and
11 mole-% water[15] or a mixture of about 96 volume percent ethanol and 4 % water
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Water is the chemical substance with chemical formula H2O: one molecule of water
has two hydrogen atoms covalently bonded to a single oxygen atom.
• The boiling point of water (and all other liquids) is directly related to the
barometric pressure. For example, on the top of Mt. Everest water boils at
about 68 °C (154 °F), compared to 100 °C (212 °F) at sea level. Conversely,
water deep in the ocean near geothermal vents can reach temperatures of
hundreds of degrees and remain liquid.
• Water has a high surface tension caused by the weak interactions, (Van Der
Waals Force) between water molecules because it is polar. The apparent
elasticity caused by surface tension drives the capillary waves.
• Water also has high adhesion properties because of its polar nature.
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partly frozen pond because the water on the bottom has a temperature of
around 4 °C (39 °F).
Property Value
Molar mass 18.015
Molar Volume 55.5 moles/liter
Boiling Point (BP) 100°C at 1 atm
Freezing point (FP) 0°C at 1 atm
Triple point 273.16 K at 4.6 torr
Surface Tension 73 dynes/cm at 20°C
Vapor pressure 0.0212 atm at 20°C
Heat of vaporization 40.63 kJ/mol
Heat of Fusion 6.013 kJ/mol
Heat Capacity (cp) 4.22 kJ/kg.K
Dielectric Constant 78.54 at 25°C
Viscosity 1.002 centipoise at 20°C
Density 1 g/cc
Density maxima 4°C
Specific heat 4180 J kg-1 K-1 ( T=293…373 K)
Heat conductivity 0.60 W m-1 K-1 (T=293 K)
Melting heat 3.34 x 105 J/kg
Evaporation heat 22.6 x 105 J/kg
Critical Temperature 647 K
Critical pressure 22.1 x 106 Pa
Speed of sound 1480 m/s (T=293 K)
Relative permittivity 80 (T=298 K)
• Water is miscible with many liquids, for example ethanol, in all proportions,
forming a single homogeneous liquid. On the other hand, water and most
oils are immiscible usually forming layers according to increasing density
from the top. As a gas, water vapor is completely miscible with air.
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Chapter 4
The permeate is finally collected in the liquid state after condensation. The
liquid product is rich in the more rapidly permeating component of feed mixture.
The retentate is made up of the feed materials that cannot pass through the
membrane.
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A porous stainless steel sintered disc used as support for the membranes was
fixed in a rubber o-ring. This rubber o-ring was places in the groove in the permeate
compartment. The PVA membrane is placed on porous stainless steel sintered disk
and sealed with rubber o-ring. Vacuum on the downstream face of the membrane
was generated using a vacuum pump. A condenser was used to trap ethanol and
water vapours from the permeate compartment.
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Niacin was first described by Weidel in 1873 in his studies of nicotine. The
original preparation remains useful: the oxidation of nicotine using nitric acid.
Niacin was extracted from livers by Conrad Elvehjem who later identified the
active ingredient, then referred to as the "pellagra-preventing factor" and the "anti-
blacktongue factor." When the biological significance of nicotinic acid was
realized, it was thought appropriate to choose a name to dissociate it from nicotine,
in order to avoid the perception that vitamins or niacin-rich food contains nicotine.
The resulting name 'niacin' was derived from nicotinic acid + vitamin. Niacin is
referred to as Vitamin B3 because it was the third of the B vitamins to be
discovered. It has historically been referred to as "vitamin PP."
Severe deficiency of niacin in the diet causes the disease pellagra, where as
mild deficiency slows the metabolism, causing decreased tolerance to cold. Dietary
niacin deficiency tends to occur only in areas where people eat corn (maize), the
only grain low in niacin, as a staple food, and that do not use lime during meal/flour
production. Alkali lime releases the tryptophan from the corn in a process called
nixtamalization so that it can be absorbed in the intestine, and converted to niacin.
The recommended daily allowance of niacin is 2-12 mg/day for children, 14 mg/day
for women, 16 mg/day for men and 18 mg/day for pregnant or breast-feeding
women.
4.3 PROPERTIES:
1. Anti pellagra vitamin.
2. Colorless or white crystalline powder.
3. Soluble in water and boiling alcohol.
4. Insoluble in most lipid solvent.
5. No hygroscopic and stable in air.
6. It is resistant to heat, oxidation and alkalis.
7. It is in fact, one of the most stable vitamins.
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Niacin, when taken in large doses, blocks the breakdown of fats in adipose
tissue, thus altering blood lipid levels. Niacin is used in the treatment of
hyperlipidemia because it reduces very-low-density lipoprotein (VLDL), a
precursor of low-density lipoprotein (LDL) or "bad" cholesterol. Because niacin
blocks breakdown of fats, it causes a decrease in free fatty acids in the blood and, as
a consequence, decreased secretion of VLDL and cholesterol by the liver. By
lowering VLDL levels, niacin also increases the level of high-density lipoprotein
(HDL) or "good" cholesterol in blood, and therefore it is sometimes prescribed for
patients with low HDL, who are also at high risk of a heart attack. Niacin is
sometimes consumed in large quantities by people who wish to fool drug screening
tests, particularly for lipid soluble drugs such as marijuana. It is believed to
"promote metabolism" of the drug and cause it to be "flushed out." Scientific
studies have shown it does not affect drug screenings, but can pose a risk of
overdose, causing arrhythmias, metabolic acidosis, hyperglycemia, and other
serious problems.
4.4 TOXICITY
People taking pharmacological doses of niacin (1.5 - 6 g per day) often
experience a syndrome of side-effects that can include one or more of the
following:
Dermatological complaints.
Facial flushing and itching.
Dry skin.
Skin rashes including acanthosis nigricans .
Gastrointestinal complaints.
Dyspepsia (indigestion).
Liver toxicity.
Fulminant hepatic failure.
Hyperglycemia.
Cardiac arrhythmias.
Birth defects.
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4.5 BIOSYNTHESIS
The liver can synthesize niacin from the essential amino acid tryptophan,
requiring 60 mg of tryptophan to make one mg of niacin. The 5-membered aromatic
heterocycle of tryptophan is cleaved and rearranged with the alpha amino group of
tryptophan into the 6-membered aromatic heterocycle of niacin.
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vegetables, and cereal grains. Dietary tryptophan is also converted to niacin in the
body. Vitamin B3 is often found in combination with other B vitamins including
thiamine, riboflavin, pantothenic acid, pyridoxine, cyanocobalamin, and folic acid.
Niacin, taken orally as nicotinic acid, can produce redness, warmth, and
itching over areas of the skin; this "niacin flush" usually occurs when doses of 50
mg. or more are taken and is a result of the release of histamine by the cells, which
causes vasodilation. This reaction is harmless; it may even be helpful by enhancing
blood flow to the "Flushed" areas, and it lasts only 10-20 minutes. When these
larger doses of niacin are taken regularly, this reaction no longer occurs because
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stores of histamine are reduced. Many people feel benefit from this "flush," but if it
is not enjoyable, supplements that contain vitamin B3 in the form of niacinamide or
nicotinamide can be used, as they will not produce this reaction. (Note: When
vitamin B3 is used to lower cholesterol levels, the nicotinic acid form must be used;
the niacinamide form does not work for this purpose.)
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Niacin is important for proper blood circulation and the healthy functioning of the
nervous system.
It maintains the normal functions of the gastro-intestinal tract and is essential for the
proper metabolism of proteins and carbohydrates.
Niacin dilates the blood vessels and increases the flow of blood to the peripheral
capillary system.
This vitamin is also essential for synthesis of the sex hormones, namely, oestrogen,
progesterone, and testosterone, as well as cortisone, thyroxin, and insulin.
Nicotinamide
can be used instead
of nicotinic acid. As we can see from these two structural formulae they are almost
the same.
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Humans do not have the ability to synthesise sufficient nicotinic acid, this
means that it is an essential component of a balanced diet. Some mammals are able
to synthesise this chemical so it is not an essential component of their diets. For
example, dogs can synthesise nicotinic acid from the amino-acid tryptophan. This
might be an essential amino-acid, but for dogs, nicotinic acid is definitely NOT a
vitamin. Bacteria in our large intestines, the colon, may convert tryptophan into
nicotinic acid; this means that we could survive if sufficient bacterial activity took
place. Our intestinal bacteria would require 60 mg of tryptophan to synthesise 1 mg
of nicotinic acid so don't count on them.
4.10 SOURCES
Nicotinic Acid is found in milk, yeast, eggs, etc. Here is a table of average
values for the Nicotinic Acid content of a variety of foods.
Food Content mg/100gg/10gm
Meat Extract 60.0
Marmite 58.5
Roast Beef 5.0
Sardines in Oil 5.0
Kippers 4.2
Whole meal Bread 3.5
Beer 0.7
Boiled Cabbage 0.15
Milk 0.08
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1. Mix about 100 mg with 1 ml of dil NaOH solution & boil, no ammonia is
evolved (distinction from nicotinamide).
2. Mix about 100 mg with 10mg of citric acid & 3 drops of acetic anhydride
& heat on a water bath, a red – violet colour is produced.
4.14 PRECAUTIONS:
The use of large doses of niacin for long periods causes release of
histamine. This in turn can cause severe flushing, severe itching of the
skin and gastro intestinal disturbances.
If taken in does of 3gm per day, niacin has been reported to cause
elevation of uric acid in the blood and glucose.
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Niacin, specifically the form of niacinamide, has also been shown to provide
relief with complications resulting from diabetes. In a recent clinical study
54
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consisting of 343 individuals without diabetes and 125 with the disease, roughly
3000 milligrams per day were administered. Hemoglobin A1C (a particular
measure of blood sugar over a period of time) actually decreased in the diabetic
group over a 60-week follow-up period. Further research is needed on niacinamide,
but intial studies indicate its potentiality in the treatment of arthritis. In addition,
Vitamin B3 may reduce inflammation, increase joint mobility, and may also aid in
cartilage repair.
Taking niacin with food may reduce stomach upset and the risk of stomach
ulcer. Doses are usually started low and gradually increased to minimize the
common side effect of skin flushing. Taking aspirin or non-steroidal anti-
inflammatory drugs (NSAIDs) at the same time during the first one to two weeks
may reduce this flushing. Use of an antihistamine 15 minutes prior to a niacin dose
may also be helpful. The flushing response may decrease on its own after one to
two weeks of therapy. Extended release niacin products may cause less flushing
than immediate release (crystalline) formulations, but may have a higher risk of
stomach upset or liver irritation. In general, not all niacin products are equivalent.
Patients switching from one product to another may have an increase or decrease in
side effects.
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Chapter 5
IMPORTANTS OF NIACIN
Niacin deficiency symptoms can be seen in diets with niacin intake below
7.5 mg. per day, but often this is not the only deficiency; vitamin B1, vitamin B2,
and other B vitamins, as well as protein and iron may be low. To treat pellagra and
niacin deficiency disorders, vitamin B3 supplements should be taken along with
good protein intake to obtain adequate levels of the amino acid tryptophan. As
described earlier, about 50 % of daily niacin comes from the conversion in our liver
of tryptophan to niacin with the help of pyridoxine (vitamin B6).
5.1 REQUIREMENTS:
Many food charts list only sources that actually contain niacin and do not
take into account tryptophan conversion into niacin. Approximately 60 mg. of
tryptophan can generate 1 mg. of niacin. But tryptophan is available for conversion
only when there are more than sufficient quantities in the diet to synthesize the
necessary proteins as tryptophan are used in our body with the other essential amino
acids to produce protein.
Niacin needs are based on caloric intake. We need about 6.6 mg. per
1,000 calories, and no less than 13 mg. per day. Women need at least 13 mg. and
men at least 18 mg. per day and for children ranges from 9-16 mg.
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not uncommon as a therapeutic dose. The other B vitamins should also be supplied
so as to not create an imbalanced metabolic condition.
For example, the use of lime (as in limestone, the mineral, not lime juice in
the fruit) can help release vitamin B3 from corn and make it available for
absorption. Native American food practices that involve the addition of ash from
cooking fires ("pot ash" or "potash") to corn-based recipes are one type of cooking
technique that helps make vitamin B3 available for absorption.
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59
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Researchers from the Chicago Health and Aging Project interviewed 3,718
Chicago residents aged 65 or older about their diet, then tested their cognitive
abilities over the following six years. Those getting the most niacin from foods (22
mg per day) were 70% less likely to have developed Alzheimer's disease than those
consuming the least (about 13 mg daily), and their rate of age-related cognitive
decline was significantly less. In addition to eating the niacin-rich foods, another
way to boost our body's niacin levels is to eat more foods rich in the amino acid
tryptophan. Our body can convert tryptophan to niacin, with a little help from other
B vitamins, iron and vitamin C. Foods high in tryptophan include shrimp, crimini
mushrooms, yellow fin, tuna, halibut, chicken breast, scallops, salmon, turkey and
tofu. As we can see, several foods rich in tryptophan provide two ways to increase
niacin levels as they are also rich in the B vitamin. (August 23, 2004)
The term "niacin," often used interchangeably with the term "vitamin B3," is
a non-chemical term that can actually refer to several different forms of the vitamin.
Most often, "niacin" is used to refer to "nicotinic acid," the form of vitamin B 3 with
documented cholesterol-lowering potential. This form of the vitamin also carries
with it the greatest risk of side effects. Supplements focused on cholesterol
reduction and alteration of fat metabolism typically include vitamin B3 in the form
of nicotinic acid. The nicotinamide form of vitamin B3 is also widely available in
supplement form. This chemical form of vitamin B3 carries a much lower risk of
side effects and is commonly used in supplement formulas designed to support
health in conditions not involving cholesterol excess or altered fat metabolism.
Particularly in formulas for pregnancy or in children's formulas, the nicotinamide
version is often preferred. Many formulas include both forms of vitamin B3, with
small amounts of nicotinic acid and larger amounts of nicotinamide.
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nutrients. The following chart shows the World's Healthiest Foods that are either an
excellent, very good, or good source of vitamin B3 (niacin). Next to each food
name, we shall find the serving size we used to calculate the food's nutrient
composition, the calories contained in the serving, the amount of vitamin B3
(niacin) contained in one serving size of the food, the percent Daily Value (DV%)
that this amount represents, the nutrient density that we calculated for this food and
nutrient, and the rating we established in our rating system. For most of our nutrient
ratings, we adopted the government standards for food labeling that are found in the
U.S. Food and Drug Administration's "Reference Values for Nutrition Labeling."(25)
World's Healthiest Foods ranked as quality sources of:vitamin B3 (niacin)
World's
Nutrien
Serving Amount DV Healthiest
Food Cals t
Size (mg) (%) Foods
Density
Rating
Crimini mushrooms, 26.
5 oz-wt 31.2 5.39 15.6 Excellent
raw 9
Tuna, yellowfin, 157. 67.
4 oz-wt 13.54 7.7 Excellent
baked/broiled 6 7
Tamari (Soy Sauce) 1 tbs 10.8 0.72 3.6 6.0 Good
Chicken breast, 223. 72.
4 oz-wt 14.41 5.8 very good
roasted 4 0
187. 48.
Calf's liver, braised 4 oz-wt 9.61 4.6 very good
1 0
Halibut, 158. 40.
4 oz-wt 8.08 4.6 very good
baked/broiled 8 4
Asparagus, boiled 1 cup 43.2 1.95 9.8 4.1 very good
Salmon, chinook, 261. 56.
4 oz-wt 11.34 3.9 very good
baked/broiled 9 7
179. 38.
Venison 4 oz-wt 7.61 3.8 very good
2 0
Romaine lettuce 2 cup 15.7 0.56 2.8 3.2 Good
229. 38.
Lamb loin, roasted 4 oz-wt 7.75 3.0 Good
1 8
214. 36.
Turkey breast, roasted 4 oz-wt 7.22 3.0 Good
3 1
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Chapter 6
MATERIAL BALANCE
1 Kg of Raw tobacco
∴ Wet slurry = 6 Kg
0.05 X 1000 = X
∴ X = 50 gm
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6.1.2 Filtration:-
Wet Tobacco
Wet slurry [i.e.4Kg wet tobacco]
Filtration
(6 Kg)
Filtrate
(1400 ml)
Loss = 600 ml
The wet tobacco after filtration can be dried and send to the cigarette
manufacturing unit to get non addictive cigarette.
Nicotine Solution
1400 ml of Steam 1040 ml
Distillation
Filtrate
Waste
360 ml
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6.1.4 Separation:-
Nicotine layer
33ml of HNO3
Reaction
33ml of Reactor Product
110-115 0 C
Nicotine 30 min Niacin,
Methylamine;
Oxalic acid &
CO2
The product from oxidation reaction in the form of precipitate was kept in
the accumulator for near about half hour. In the accumulator there was formation of
two layers due to density difference, the lower layer of Oxalic acid and upper layer
of Nicotinic acid, which was send to dryer.
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Top Nicotinic
acid
(45 gm) layer (36 gm)
Accumulator
Reaction
Product
Bottom Oxalic
acid
layer (9 gm)
Overall material balance
Reaction product = Top Nicotinic acid layer + Bottom Oxalic acid layer
6.1.6 Drying:-
Moisture removed
Let X and Y are the gm of water removed and product Niacin obtained.
36 = X+Y
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Solid balance
0.8 X 36 = 0.95 Y
Y = 30 gm
Nicotinic acid = 30 gm
X = 6 gm
Moisture removed = 6 gm
(18)
6.2 ENERGY BALANCE
Amount of heat required to raise the temperature of tobacco mixture in mixing tank
from room temp. (i.e. 300C) to 600C
Q = m Cp ∆ T
Q = 6 X Cp X (60-30)
Approximate Specific heat capacity (Cp) values can be calculated for solids
and liquids by using a modified form of Kopp’s law, which is given by Werner
(1941). (19)
H 14 14 X 9.6 = 134.4
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N 28 28 X 26.0 = 728.0
162 1762.4
1762.4
Capacity 162
∴ Q = 6 X 10.88 X 30 = 1958.4 KJ
Steam in
Condensate
Amount of heat required in steam distillation section.
Q = m Cp ∆ T
Q = 1249.024 KJ/hr
Q = mCp ∆ T
1249.024 = m X 1 X (110-28)
∴ m = 15.232 kg/hr
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33mlofHNO3
Q = mCp ∆ T
Q = 0.066X10.88 X (110-30)
Q = 57.4464 KJ /hr
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Chapter 7
REACTOR DESIGN
For 33 lit. of total reaction mixture.
V = 33 lit.
= 33 lit.
∴ V = 33 X 10-3 + 10 % Excess
∴ V = 36.3 X 10-3 m3
∴ Area of = π D2
Reactor 4
For plate thickness up to 50 mm (16)
L = 6
D
∴ Length of reactor = L = 6 D
∴ Volume = π D 2 X 6 D
4
∴ V = 1.5π D3
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36.3X10-3 = 4.712 D 3
∴ D 3 = 7.7X 10-3
∴ D = 0.19 m
Di = 20 cm ≈ 200mm
Since L = 6
D
∴ L = 6 D = 6 X 20 = 120 cm
L = 1.2 m
P = 1atm
=101.325 X103 N/m2
Thickness is t = PD +C
D= 0.2 m
2fJ F = For Steel plate
The steel plate IS : 2041- 1962 allowable stress
3 3 = 3.5 X 106N/m2
= 101.325 X 10 X 0.2 + 1 X 10
J = 80%
2 X 3.5X106X 0.80
t = 4.62 mm ≈ 5mm
v = t [π DL + π D 2 ]
2
-3
v = 5X 10 [0.754 +0.063]
v= 40.8 X 10-3 m3
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1.009 = Nicotine
1 gm/cm3
Density of HNO3
∴ 1.502 = ------------------
Density of H2O
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m 189 Kg
Volume of HNO3 = -------- = --------- = --------- = 0.1258 m3
1502 Kg/m3
So for carrying oxidation reaction, take 1.6 ml of Nicotine & 1.25 ml HNO3
to get the desired product i.e. Nicotinic acid (Niacin). (18)
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Chapter 8
COST ESTIMATION
8.1 COST OF EQUIPMENT:-
Sr.No Item Uni Cost / Total
. t Unit Cost(Rs.)
1 Pulverizer 1 200000 200000
2 Mixing Tank 1 3200000 320000
3 Filter press 1 480000 480000
4 Storage Tank 4 4000 16000
5 Steam Distillation 1 500000 500000
Setup
6 Condensor 1 100000 100000
7 Reactor 1 25000 25000
8 Dryer 1 150000 150000
Total ( E ) 1791000
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= 5397170 + 1028034
= Rs. 6425204
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= Rs. 58839
= Rs. 1765170
8.3.2 Utilities:-
a) Water:-
b) Steam:-
c) Electricity:-
= Rs. 1089000
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= 0.3 X 77000
= Rs.23100
= 0.1 X78925
= Rs.7893 /month
= 0.005 X 5397170
A) Direct production cost = Raw material cost + Cost of Utilities + Operating Cost
+ Lab
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= 0.02 X 5397170
= Rs. 107943
C) Insurance = 1 % FCI
= 0.01 X 5397170
= Rs. 53972
= 0.2 X 78925
= Rs.15785
= 0.01 X 5397170
= Rs. 53972
= Rs.3199646
= 45 X 30 = 1350 Kg / month
= 40500 Kg / month
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Sale:- (14)
Monthly Sale:-
Niacin = 1350 X 2100 = Rs. 2835000
Oxalic acid = 1350 X 280 = Rs. 378000
Tobacco = 40500 X 15 = Rs. 607500
Total monthly sale = 2835000 + 378000 +607500
= Rs. 3820500
Gross profit = Total monthly sale - Total monthly production cost
= 3820500 – 3199646
= Rs. 620854
Income tax = 40 % Gross profit
= 0.4 X 620854
= Rs. 248342
Net profit = Gross profit – Income tax
= 620854 – 248342
= Rs. 372512 /month = 372512 X 12 = Rs. 4470144 /year
Rate of return on investment = Net profit per year
Fixed Capital Investment
= 4470144
5397170
= 0.83
Rate of return = 0.83
This evaluation is based on laboratory readings & previous literature on Niacin, so
before going for large scale production a test on pilot plant is necessary. (14)
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Chapter 9
PLANT LAYOUT
After the process flow diagram was completed and before detailed piping
design and layout can begin, the layout of process unit must be planned and
equipment within these process unit must be planned. This layout can play an
important role in determining constructing and manufacturing cost; and thus must
be planned carefully. Good plant layout keeps safety, appearance, convenience,
overall cost, erecting cost, operating and maintenance cost to the minimum. Safety
and optimum utilization of available area should be given prime importance in plant
layout. The key to economical construction and efficient operation is a carefully
planned functional agreement of equipment, piping and building. An accessible and
aesthetically pleasing plot plan can make major contribution to safety, employee
satisfaction and sound community relation.
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Storage Layout:-
Raw material storage tank should be located such that the transportation to
the process area is done easily loaded and unloaded.
Equipment Layout:-
Safety: -
Fire station should be located nearer to process area. In every unit hose
pipes, fire extinguisher should be placed.
Plant Expansion: -
Utilities: -
Administrative building: -
This should be located at the entrance of the main gate of the factory and
there must be provision made for communicating with every plant.
These should be located near the process plant. Due to which the evaluation
results and hence correction can be easily done within no time.
Commodities: -
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Parking and canteen should be located near to the unit but not too close to
the unit. They should be separated from actual plant by the road.
Security Office: -
The security office and time office (checkers gate) should be located near to
the entrance of the factory.
Market Area: -
Raw material required for production of Nicotinic Acid i.e. Waste Tobacco
was collected from tobacco farming nearby area and also from tobacco processing
industries.(13)
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Chapter 10
CONCLUSION
Nicotinic acid is an antipellagra factor is a group of vitamin B3 . Majority
sources of it are Yeast, Rice polishing, Meatextract & Tobacco. By oxidation of
tobacco with the help of HNO3, nicotine is converted to nicotinic acid (Niacin).
With this treatment to tobacco the addictive nature of man towards tobacco
becomes non-addictive & also provide an improved tobacco product, so that blood
plasma nicotine level resulting about 0 to 5 nanograms /ml. The main aim is to go
for experimental work in lab-scale for conversion of Nicotine to Nicotinic acid from
Tobacco.It is a two step process,firstly Extraction of nicotine from tobacco and
secondly conversion of nicotine to nicotinic acid. The reactor was to be designed
for this oxidation process and the analysis of product & by- products was to be
carried out.
The objective of the process is to get non addictive tobacco product, the
poisonous Nicotine is converted to Vitamin B3, and to reduce the Carcinogenic
effect of tobacco on human health i.e. to get alternate use of tobacco for Nicotine
Sulphate (as pesticide), Niacin (Vitamin B3) pharmaceutical product, etc.
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nicotine. From 2nd Oct. 2008 it was banned to smoke at public places and also at
work places by the Government. Nicotine could also be removed from combustion
tobacco products. Alternatively nicotine-replacement therapies may be used. One
should avoid smoking by inhalation either actively or passively
FUTURE PROSPECTS
1. With the help of this treatment to the tobacco the addictive nature of tobacco
due to Nicotine becomes non-addictive.
4. We can convert the harmful nicotine to the niacin which was pharmaceutical
product.
5. For the waste coming from the tobacco industries & also from tobacco farming,
this was the important technique to get the valuable product.
6. The treated tobacco can also be used as a fertilizer for the farming purpose.
7. The main aim is to get alternative use of tobacco for Farmers due to the ban of
tobacco for beedi, hooka, chewing etc. by the Government.
8. To treat one cancer patient approximately Rs. 3.5 lacks required and near about
7.5 lacks people die due to cancer from tobacco, this can be avoided.
10. By this method we can convert waste tobacco to the valuable pharmaceutical
product
11. By optimizing the process the yield of Niacin from tobacco can be increased.
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REFERENCES
1. Agarwal O.P. “Chemistry of Organic Natural Product”(2004) Volume I,
Himalaya Publishing House, (p.280,281).
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15. Warren L. McCabe, J.C. Smith, Peter Harriott, “Unit Operations of Chemical
Engineering V th ed. (1993) McGraw Hill Book Co. Singapore (p.614, 615).
st
16. Dr. S.D. Dawande “ Process Design of Equipments” I ed. (1999),
Central Techno Publications,Nagpur-12 (p.19,20).
rd
17. Robert E. Treybal “Mass– Transfer Operations”III ed. (1981)
McGraw-Hill Book Co. Singapore (p.717, 718,719).
18. Bhatt B.I. & Vora S.M. “Stoichiometry” III rd ed. (1998) Tata Mc Graw
Hill Publishing Company Ltd. (p.66, 67,187).
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INDEX
Introduction to pervaporation 1
1.2MEMBRANE BASED PERVAPORATION SEPARATION:.........................3
.................................................................................................................................6
Literature survey 14
2.1 SEPARATION PRINCIPALS........................................................................14
2.2 PERVAPORATION THEORY..................................................................15
...........................................................................................................................21
...........................................................................................................................22
2.5 SUMMARY OF THE INVENTION .............................................................35
ETHANOl - WATER SEPARATION BY PERVAPORATION 37
3.1 EHANOL ASPECTS:-...................................................................................37
3.3 Process Description:- .....................................................................................42
experimental set-up & process 43
4.1 PERVAPORATION SYETEM......................................................................43
...............................................................................................................................43
4.2 Dietary needs..................................................................................................45
4.3 Properties: .....................................................................................................45
4.3 Pharmacological uses:-...................................................................................45
4.4 Toxicity...........................................................................................................46
4.5 Biosynthesis....................................................................................................47
4.6 Physical Properties of Nicotinic Acid (11).....................................................48
4.7 Functions of Vitamin B3 Niacin:-...................................................................50
4.8 Chemical Structure (25)..................................................................................50
4.9 Biological Synthesis .......................................................................................50
4.10 Sources..........................................................................................................51
4.11 Source Categories:........................................................................................52
4.12 Deficiency Disease:......................................................................................52
4.13 Identification Tests for NIACIN (2).............................................................52
4.14 Precautions:...................................................................................................52
4.14 Niacin Analogues:-.......................................................................................53
4.15 Vitamin B3 Uses...........................................................................................54
IMPORTANTS OF NIACIN 56
5.1 Requirements: ...............................................................................................56
5.2 Function of vitamin B3...................................................................................58
5.3 Metabolism of Fats .......................................................................................58
5.4 Support of genetic processes...........................................................................58
5.5 Deficiency Symptoms.....................................................................................59
5.6 Toxicity Symptoms.........................................................................................59
5.7 Factors that Affect Function...........................................................................59
5.8 Niacin Protects against Alzheimer's disease and Age-related Cognitive
Decline..................................................................................................................59
5.9 FORMS in Dietary Supplements....................................................................60
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LIST OF TABLE
92