The document discusses various separation processes that utilize external forces including centrifugation, thermal diffusion, electrolysis, electrodialysis, and electrophoresis. Thermal diffusion uses a temperature gradient to separate isotopes based on their slight weight differences, causing lighter isotopes to diffuse toward the hot surface and heavier ones toward the cold surface. Electrolysis uses an electric current to drive chemical reactions like chlorine and hydrogen gas production. Electrodialysis removes ions from solution using ion-selective membranes and an electric field. Electrophoresis separates charged particles like proteins and nucleic acids in a gel matrix using an electric field.
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▪ External fields can take advantage of differing degrees of response of molecules and
ions to force fields.
▪ Special note: Filtration and Centrifugation are studied in Mechanical – Physical
Separations
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▪ Thermal diffusion utilizes the transfer of heat across a thin liquid or gas to
accomplish isotope separation.
▪ The ESA → Thermal Gradient
▪ The process exploits the fact that the isotopes are either lighter and heavier.
▪ Expect a heavier stream and a lighter Stream.
▪ The molecules will diffuse towards the hot surface.
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▪ The most common examples is 235U separation of isotopes.
▪ The lighter 235U gas molecules will diffuse toward a hot surface, and the heavier 238U gas
molecules will diffuse toward a cold surface.
▪ The S-50 plant at Oak Ridge, Tennessee was used during World War II to prepare feed
material for the EMIS process.
▪ It was abandoned in favor of gaseous diffusion.
▪ This process has been used to enhance separation of isotopes in permeation processes.
▪ Water contains 0.000149 atom fraction of deuterium.
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▪ Electrolysis is a technique that uses a direct electric current
(DC) to drive an otherwise non-spontaneous chemical reaction.
▪ The ESA → Electric Current
▪ Electrolysis is commercially important as a stage in the
separation of elements from naturally occurring sources such as
ores using an electrolytic cell.
▪ The voltage that is needed for electrolysis to occur is called the
decomposition potential.
▪ In many cases, a Membrane will be used
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▪ Membrane electrolysis is a process whereby both electrode
reactions
▪ the cathodic reduction
▪ the anodic oxidation
▪ Both are linked to the transport and transfer of charged ions.
▪ In membrane electrolysis:
▪ the electrode reaction is essential to the actual separation
process.
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▪ The purpose of the membrane is to:
▪ separate the anode loop (anolyte) from the cathode loop (catholyte) by a fluid
▪ This avoids unwanted secondary reactions
▪ this combines the electrode reaction with a separation step or to isolate separately the products formed on the
electrode.
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▪ In water electrolysis:
▪ such products may be in a gaseous form such as oxygen and hydrogen as well as the acids (H+) and bases
(OH-)
▪ These are formed on the electrode or the combination of gaseous chlorine and caustic soda solution and
hydrogen as in sodium chloride electrolysis
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▪ Check this video:
▪ https://www.youtube.com/watch?v=ueeHNwL5lSE
▪ Chlorin-Caustic Soda Production
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▪ In electrodialysis
▪ Cation-permeable AND anion-permeable membranes
carry a fixed charge
▪ This prevents migration of species of like charge.
▪ The main goal is to remove ions from solution:
▪ Decrease concentration of a solute
▪ Remove a solute completely
▪ Main focus is the SOLVENT/Solution
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▪ It involves the migration of ions through ion-
exchange membranes in an applied electric field.
▪ The flux of an ion through the membrane is
dependent upon its charge, the bulk concentration
of the ion and its mass transport to the membrane
surface.
▪ In this way species can be removed from reaction
mixtures and waste streams thereby reducing the
need for costly disposal and purification.
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▪ Electrodialysis dates back to the early 1900s
▪ The GOAL → Electrodes and a direct current were used to increase
the rate of dialysis.
▪ Today:
▪ Electrodialysis refers to an electrolytic process for separating an
aqueous, electrolyte feed into:
▪ Concentrate
▪ Dilute / desalted water diluate
▪ ESA → Electric field AND ion-selective membranes
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▪ There can be many sections which are
separated depending on the type of
membrane:
▪ Example four ion-selective membranes are of two
types arranged in an alternating-series pattern.
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▪ The cation-selective membranes (C) carry
a negative charge, and thus attract and
pass positively charged ions (cations),
while retarding negative ions (anions).
▪ The anion-selective membranes (A) carry
a positive charge that attracts and
permits passage of anions.
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▪ Both types of membranes are impervious
to water.
▪ The net result:
▪ Both anions and cations are concentrated in
compartments:
▪ 2 and 4
▪ From which concentrate is withdrawn
▪ Ions are depleted in compartment 3
▪ From which the diluate is withdrawn.
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▪ Compartment pressures are essentially
equal.
▪ Compartments 1 and 5:
▪ contain the anode and cathode (respectively)
▪ A direct-current voltage causes:
▪ current to flow through the cell by ionic
conduction
▪ from the cathode (right)
▪ to the anode (left)
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▪ Both electrodes are chemically neutral
metals
▪ Typically:
▪ Anode is stainless steel
▪ Cathode platinum- coated tantalum,
niobium, or titanium.
▪ The electrodes are neither:
▪ oxidized nor reduced.
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▪ Electrodialysis:
▪ Production of table salt from seawater
▪ Concentration of brines from reverse osmosis
▪ Treatment of wastewater from electroplating
▪ De-mineralisation of cheese whey
▪ Production of ultrapure water for semiconductor industry
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▪ Check out this video:
▪ https://www.youtube.com/watch?v=wcb8RFWa6BY
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▪ Electrophoresis (from the Greek "ηλεκτροφόρηση" meaning "to bear electrons")
▪ is the motion of dispersed particles relative to a fluid under the influence of a spatially
uniform electric field.
▪ ESA → Electric Field
▪ It involves the size- and charge-based separation of charged solutes that move in
response to an electric field applied across an electrophoretic medium.
▪ The Electrophoresis of a:
▪ positively charged particles (cations) → cataphoresis
▪ negatively charged particles (anions) → anaphoresis.
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▪ It commonly occurs in a gel matrix of synthetic or natural
polymer.
▪ It must be done in a developed in-place between parallel glass
plates or inside a silica capillary to minimize electro-osmosis and
resistive Joule heating.
▪ Common Examples:
▪ Agarose
▪ Polyacrylamide
▪ Starch → its high water content allows allows passage of large solutes
through their porous structures.
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▪ Several electrophoretic modes are widely used to isolate and
concentrate biomolecules.
▪ They are distinguished by:
▪ Denaturants
▪ Matrix pH
▪ Electrolyte content relative to the direction of the applied field
gradient
▪ all of which influence the electrophoretic mobility of the
biomolecule.
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▪ It can be used to exploit the different migration velocities of charged colloidal or suspended
species in an electric field.
▪ Positively charged species, such as
▪ Dyes, hydroxide sols, and colloids, migrate to the cathode
▪ Negatively charged particles:
▪ Such as most small, suspended particles go to the anode.
▪ By changing from an acidic to a basic condition:
▪ migration direction can be changed, particularly for proteins.
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▪ Electrophoresis is thus a versatile method for separating biochemicals.
▪ Chemical stains, fluorescence, immunological probes, and spectroscopy/spectrometry are
used to visualize and recover biomolecules distinguished by electrophoresis.
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▪ From beets to sugar
If you were to measure the time it takes to produce shimmering white sugar crystals
from a beet that had just been delivered from the field to the factory, you would be
surprised:
▪ On average, it takes less than eight hours.
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▪ Juice extraction
The beets are:
▪ sliced into thin strips
▪ preheated in a cossette scalder
▪ sent to an extraction tower.
▪ Water at 70° Celsius is poured
through the device to extract the
sugar and produce raw juice.
▪ The used cosettes are dried by
means of screw presses and hot
air.
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▪ Juice purification
▪ A lime kiln is used to produce the
natural substances lime and
carbon dioxide, which are added
sequentially to the raw juice to
bind and precipitate out the non-
sugar impurities.
▪ A clear, thin juice with a sugar
content of about sixteen percent
remains.
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▪ Crystallization
▪ The thick juice is boiled until crystals are
formed, which are a glowing golden yellow
color because they are covered with syrup.
▪ The syrup is separated from the crystals in a
centrifuge.
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▪ Crystallization
▪ Hot water is used to rinse off any residual
syrup.
▪ The remaining sugar crystals are clear as
glass, and the light refracted from them is
white as snow.
▪ This sugar is dissolved and re-crystallized to
produce refined sugar – sugar that is
extremely pure.
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▪ Converting
▪ The finished sugar is dried, cooled and stored in silos, and is subsequently withdrawn and further
processed or packed.
▪ Over eighty percent of the sugar is shipped to the converting industry, which uses it to make
confectioneries, beverages, baked goods, etc.
▪ Just under twenty percent of the sugar is converted to various types of household sugar and
packaged.
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▪ Recycling
▪ All the by-products of this process are returned to the natural cycle.
▪ The pressed slices of sugar beet are used as animal feed.
▪ The Carbokalk (carbolic lime) that is a by-product of processing the juice is an excellent
fertilizer.
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▪ Leaching →
▪ the process of extracting substances from a solid by dissolving them in a liquid
▪ Leaching is the process of a solute becoming detached or extracted from its
carrier substance by way of a solvent.
▪ Leaching (in metallurgy)
▪ is a process widely used in extractive industry.
▪ Here, ore is treated with chemicals to convert the valuable metals within into:
▪ soluble salts
▪ impurity remain insoluble.
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▪ Technically an Extraction, since it:
▪ is a process of selectively removing a compound of interest from a
mixture using a solvent.
▪ The major difference between solid–liquid and liquid– liquid
systems:
▪ Difficulty of transporting the solid (often as slurry or a wet cake) from
stage to stage.
▪ For an extraction to be successful:
▪ the compound must be more soluble in the solvent than in the mixture.
▪ Additionally:
▪ the solvent and mixture must be immiscible
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▪ Making tea is a good example of extraction.
▪ Water is placed in contact with tea bags
▪ The "tea" is extracted from the tea leaves into
the water.
▪ This works because:
▪ the "tea" is soluble in water
▪ the leaves are not soluble
▪ A simple filtration process separates the solids vs.
aqueous material
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▪ In Leaching, there are three substances which are required:
▪ a carrier
▪ a solute
▪ and a solvent
▪ As you can see, this is a partition between 2 binary systems
▪ (at least)
▪ The main property exploited here is solubility
▪ To promote rapid solute diffusion out of the solid and into the
liquid solvent, particle size of the solid is usually reduced.
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▪ Some other type of properties which may be exploited are:
▪ Particle size
▪ Solvent
▪ Temperature
▪ Agitation
▪ Surface area
▪ Homogeneity of the carrier and solute
▪ Microorganism activity
▪ Mineralogy
▪ Intermediate products
▪ Crystal structure
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▪ Type of Operations:
▪ In the pharmaceutical, food, and natural product
industries:
▪ countercurrent solid transport is provided by complicated
mechanical devices.
▪ In adsorptive-bubble separation methods:
▪ surface-active material collects at solution interfaces.
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▪ If the (very thin) surface layer is collected:
▪ partial solute removal from the solution is achieved.
▪ In ore flotation processes:
▪ solid particles migrate through a liquid and attach to rising
gas bubbles
▪ This allows a floating out of solution.
▪ When leaching is rapid, it can be accomplished in one
stage.
▪ However, the leached solid will retain surface liquid that
contains solute.
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▪ Leaching of large solids can be very slow because of
small solid diffusivities.
▪ It is common to reduce size of the solids by:
▪ crushing, grinding, flaking, slicing, etc.
▪ Solids are contacted with solvent by:
▪ either percolation or immersion.
▪ To recover solute in the extract, it is desirable to add one or more washing stages in a
countercurrent arrangement.
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▪ When operating under Stages:
▪ Effluents from a leaching stage are essentially solids-free liquid
▪ They are called the overflow, and wet solids, the underflow.
▪ To reduce the concentration of solute in the liquid portion of the underflow:
▪ leaching is often accompanied by countercurrent-flow washing stages.
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▪ The combined process produces:
▪ A final overflow
▪ referred to as extract, which contains some of the solvent and most of the solute
▪ A final underflow
▪ the extracted or leached solids, which are wet with almost pure solvent.
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▪ Ideally:
▪ the soluble solids are perfectly separated from the insoluble solids
▪ BUT solvent is distributed to both products.
▪ Therefore, additional processing of the extract and the leached solids is necessary
to recover solvent for recycle.
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▪ Go back to the Case Study
▪ Identify the Extraction Process
▪ Is this liq-liq or solid-liq?
▪ Why do we have a slicer?
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▪ Industrial applications of leaching include:
▪ REMOVALS:
▪ Removal of copper from ore using sulfuric acid
▪ Removal of caffeine from green coffee beans using supercritical CO2
▪ RECOVERIES:
▪ Recovery of proteins and other natural products from bacterial cells.
▪ Recovery of gold from ore using sodium-cyanide solution
▪ EXTRACTIONS:
▪ Extraction of sugar from sugar beets using hot water
▪ Extraction of tannin from tree bark using water
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▪ Washing is the process of selectively removing unwanted compounds from a mixture
using a solvent.
▪ For a washing to be successful:
▪ the unwanted materials must be more soluble in the solvent than in the mixture.
▪ Additionally, the solvent and mixture must be immiscible.
▪ Immiscible solvents are not soluble in each other and form two layers when mixed.
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▪ The washing of clothes is a good example.
▪ Dirty clothes are placed in water.
▪ The dirt, the unwanted material, is removed leaving the
clothes, what we are interest in, behind.
▪ This works because the dirt is soluble in the water and
clothes are not.
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▪ When:
▪ leaching is very rapid as with small particles containing very soluble solutes
▪ or when leaching has already been completed
▪ or when solids are formed by chemical reactions in a solution
▪ We have to:
▪ counter-currently wash the solids to reduce the solute concentration in the liquid adhering
to the solids.
▪ This can be accomplished in a series of:
▪ gravity thickeners
▪ or centrifugal thickeners, called hydroclones
▪ Note that they must be arranged for countercurrent flow of the underflows and
overflows.
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▪ Combined feed to the thickener consists of:
▪ feed solids or underflow from an adjacent thickener, together with fresh solvent or
overflow from an adjacent thickener.
▪ The thickener must first thoroughly mix liquid and solids.
▪ Then, a uniform concentration of solute in the liquid is obtained
▪ Then, it must produce:
▪ an overflow free of solids
▪ an underflow with as high a fraction of solids as possible.
▪ A thickener consists of a
▪ large-diameter
▪ shallow tank
▪ a flat/slightly conical bottom.
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▪ The combined feed enters the tank near the center by means of a feed launder that
discharges into a feed well.
▪ Settling and sedimentation of solid particles occur by gravity due to a solid particle
density that is greater than the liquid density.
▪ In essence:
▪ solids flow downward
▪ liquid flows upward.
▪ Around the upper, inner periphery of the tank:
▪ Overflow launder or weir for continuously removing clarified liquid.
▪ Solids settling to the tank bottom are moved inward toward a thick sludge discharge
by a slowly rotating motor-driven rake.
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▪ Thickeners as large as 100 m in diameter and 3.5 m high have been constructed.
▪ In large thickeners, rakes revolve at about 2 rpm.
▪ Residence times of solids and liquids in a gravity thickener are often large (minutes
or hours) and
▪ These are sufficient to provide adequate residence time for mass transfer and
mixing when small particles are involved.
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▪ The FEED:
▪ pressurized feed slurry enters tangentially
▪ This creates, by centrifugal force, a downward-spiraling motion.
▪ Higher-density, suspended solids are
▪ by preference, driven to the wall
▪ This becomes conical as it extends downward
▪ The OUTLET:
▪ It is then discharged as a thickened slurry at the hydroclone bottom.
▪ The liquid, which is forced to move inward and upward as a spiraling vortex
▪ It exits from a vortex-finder pipe extending downward from the closed hydroclone top to a
location just below feed entry.
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▪ A common manufacturing step is drying
▪ Since many chemicals are processed wet but sold as dry solids
▪ The term drying also describes a gas mixture in which a condensable
vapor (i.e. water vapor) is removed from a non-condensable gas
(i.e. air) by cooling
▪ Although the only requirement is:
▪ that the vapor pressure of the liquid to be evaporated from the solid be
higher than its partial pressure in the gas stream
▪ This Section deals only with drying operations that produce solid
(dry) products.
▪ ESA → Heat
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▪ External conditions as:
▪ Temperature
▪ Humidity
▪ Air flow
▪ Degree of solid subdivision
▪ Drying rate
▪ Internal diffusion conditions must be considered as well:
▪ Capillary flow
▪ Equilibrium moisture content
▪ Heat sensitivity
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▪ It is important to note that:
▪ solid, liquid, and vapor phases coexist in drying.
▪ This is a challenge for the equipment-design.
▪ The dryer design and operation represents a complex problem.
▪ Procedures are difficult to devise
▪ Equipment size may be controlled by heat transfer rather than MT
▪ NOTE:
▪ Technically, this could be a Heat Transfer Unit as well…
▪ Use a psychrometric charts are key:
▪ adiabatic-saturation temp.
▪ wet-bulb temperature
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▪ Drying can be expensive:
▪ especially when large amounts of water, with its high heat of vaporization
▪ Water and energy conservation measures, and advances in equipment design have
broadened.
▪ The use of pre-feed dewatering operations by mechanical means, which also
diminish the length of drying cycles are:
▪ Expression
▪ Gravity, vacuum, or pressure filtration
▪ Settling
▪ Centrifugation
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▪ Heat must be transferred to the material being dried:
A. By convection from a hot gas in contact with the material
B. By conduction from a hot, solid surface in contact with the material;
C. By radiation from a hot gas or surface
D. By heat generation within the material by:
▪ dielectric, radio frequency, or microwave heating
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▪ Industrial Equipment
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▪ Rotatory Dryers
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▪ Drying is widely used to remove moisture from:
▪ crystalline particles of inorganic salts and organic compounds to produce a free-flowing
product;
▪ biological materials
▪ Such as foods
▪ pharmaceuticals
▪ detergents;
▪ lumber, paper, and fiber products;
▪ dyestuffs;
▪ solid catalysts;
▪ milk;
▪ films and coatings,
▪ products where high water content entails excessive transportation and distribution costs.
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▪ Evaporation, is defined as:
▪ the transfer of volatile components of a liquid into a gas by heat transfer.
▪ Applications include:
▪ Humidification*
▪ Air conditioning
▪ Concentration of aqueous solutions
▪ For our Separation Process Course, the latter is the one of interest
▪ NOTE: Evaporation is also commonly referred as a Heat Transfer Operation
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▪ Before crystallizing an inorganic solute from an aqueous
solution:
▪ it is customary to bring the solute concentration close to
saturation.
▪ This is accomplished by evaporating water in an evaporator.
▪ It is also used to concentrate solutions even when the solute
is not subsequently crystallized:
▪ Solutions of sodium hydroxide
▪ Industrial acids
▪ Bulk Chemical
▪ Food & Beverages
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▪ When the vapor formed is essentially pure:
▪ there is no mass-transfer resistance in the vapor.
▪ When the liquid is agitated:
▪ mass transfer is sufficiently rapid
▪ We can assume that the rate of solvent evaporation is related to:
▪ The rate of heat transfer from the
▪ Evaporators differ in configuration and degree of liquid agitation.
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▪ a) Horizontal-tube evaporator.
▪ Consists of a horizontal cylindrical vessel
▪ It is equipped in the lower section with a horizontal bundle of tubes
▪ Inside of these steam condenses and outside of which the solution to
be concentrated boils.
▪ Agitation is provided only by the movement of the bubbles leaving
the evaporator as vapor.
▪ This type of unit is suitable only for low-viscosity solutions that do
not deposit scale on the heat-transfer surfaces.
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▪ (b) Short-vertical-tube evaporator.
▪ It differs significantly from the horizontal-tube evaporator.
▪ The tube bundle is arranged vertically
▪ In this arrangement:
▪ the solution goes inside the tubes and steam condensing outside.
▪ Boiling inside the tubes causes the solution to circulate.
▪ This provides additional agitation and higher heat-transfer
coefficients.
▪ This type of evaporator is not suitable for very viscous solutions.
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▪ (c) Long-vertical-tube evaporator.
▪ The tubes are much longer.
▪ This lengthening the vertical tubes provides:
▪ a separate vapor–liquid disengagement chamber
▪ A higher liquid velocity can be achieved
▪ An even higher heat-transfer coefficient.
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▪ (d) Forced-circulation evaporator.
▪ To handle very viscous solutions:
▪ a pump is used to force the solution upward through relatively short
tubes
▪ As the name implies, it requires external Energy / Shaft Work
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▪ (e) Falling-film evaporator.
▪ It is popular for concentrating heat-sensitive solutions such as fruit juices.
▪ The solution enters at the top
▪ It then flows as a film down the inside walls of the tubes.
▪ Concentrate and vapor produced are separated at the bottom.
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▪ (d) Forced-circulation evaporator.
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▪ Drying is widely used to remove moisture from:
▪ Bulk Chemical Production
▪ Removal of water / Concentration
▪ Food & Beverage Industries
▪ Concentration of materials
▪ pharmaceuticals
▪ Paper, and fiber products
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▪ Falling Film Evaporator:
▪ https://www.youtube.com/watch?v=N7iIzKA5xh8
▪ Black Liquor Evaporator:
▪ https://www.youtube.com/watch?v=K_v4eFjCEGw
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▪ Physical Phenomena Overview:
▪ Crystallization is the process by which a solid forms:
▪ where the atoms or molecules are highly organized
▪ Its structure is called a crystal
▪ Typically forms of Crystallization:
▪ precipitating from a solution
▪ Freezing
▪ Deposition directly from a gas (rare)
▪ Attributes of the resulting crystal depend largely on factors such as:
▪ Temperature
▪ Pressure
▪ Time
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▪ Crystallization is a purification step
▪ the conditions must be such that impurities do not
precipitate with the product.
▪ Crystallization occurs in two major steps.
▪ The first is nucleation:
▪ the appearance of a crystalline phase from either a
super-cooled liquid or a supersaturated solvent.
▪ The second step is known as crystal growth
▪ which is the increase in the size of particles and
leads to a crystal state.
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▪ In solution crystallization:
▪ the mixture, which includes a solvent, is cooled and/or the solvent is evaporated.
▪ In melt crystallization:
▪ two or more soluble species are separated by partial freezing.
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▪ Crystallization is a solid–fluid separation in which crystalline
particles are formed from a homogeneous fluid phase.
▪ Ideally, crystals are pure chemicals
▪ Typically, they are obtained in a high yield with a desirable shape
▪ For formation of organic crystals, organic solvents such as:
▪ acetic acid, ethyl acetate, methanol, ethanol, acetone, ethyl ether,
chlorinated hydrocarbons, benzene, and petroleum fractions.
▪ For aqueous or organic solutions, crystallization is effected by:
▪ cooling a solution
▪ evaporating the solvent
▪ or a combination of the two.
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▪ Process Overview:
▪ Crystallization is a liquid-solid mass transfer operation
▪ Here, the solid crystals are formed
▪ They must be precipitated from solution or melt.
▪ In such separation:
▪ the substance being crystallized diffuses from liquid to solid phase
▪ It then interacts with the solid surface where the crystals grow.
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▪ Many of the impurities present in the solution are discarded during crystallization so
that the product is obtained in relatively purer form.
▪ Crystallization has been traditionally known to be the best and the cheapest
method for:
▪ obtaining pure solids from impure solutions
▪ They achieve desirable properties such as:
▪ Flow-ability
▪ Handling
▪ packaging characteristics
▪ attractive appearances
▪ Particle properties like crystal structure, crystal size distribution, polymorphism are
vital
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▪ Agitated Batch Crystallizer
▪ Swenson–Walker Crystallizer
▪ Circulating Liquor Crystallizers
▪ Circulating Magma Crystallizers
▪ Melt Crystallization
▪ Suspension Based Melt Crystallization
▪ Progressive Freezing Crystallization
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▪ Agitated Batch Crystallizer
▪ Swenson–Walker Crystallizer
▪ Circulating Liquor Crystallizers
▪ Circulating Magma Crystallizers
▪ Melt Crystallization
▪ Suspension Based Melt Crystallization
▪ Progressive Freezing Crystallization
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▪ Agitated Batch Crystallizer
▪ Swenson–Walker Crystallizer
▪ Circulating Liquor Crystallizers
▪ Circulating Magma Crystallizers
▪ Melt Crystallization
▪ Suspension Based Melt Crystallization
▪ Progressive Freezing Crystallization
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▪ Crystallization is one of the oldest known separation operations
▪ Some common applications:
▪ Recovery of sodium chloride as salt crystals from water
▪ Recovery of sugar crystals
▪ Ammonium sulphate & sodium chromate
▪ Organic and inorganic compounds are marketed as crystals.
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