UNIT

OPERATIONS

SUBMITTED TO : MR. ARUN KUMAR SUBMITTED BY : SAKET

M. PHARMACY
PHARMACEUTICAL
CHEMISTRY
DEPARTMENT OF PHARMACEUTICAL SCIENCE
GURUGRAM UNIVERSITY, GURUGRAM
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INTRODUCTIO
N
 Unit Operations gives idea about:
• specific physical operation;
• different equipment - its design,
• material of construction and operation;
• calculation of various physical parameters (mass flow, heat
flow, mass balance, power and force etc.).

Unit operations involve a physical change or chemical

transformation such as separation, crystallization, evaporation,
filtration, polymerization, isomerization, and other  reactions
EXTRACTION
 Extraction defined as the treatment of the plant or animal tissues with solvent, whereby the
medicinally active constituents or API are dissolved & most of the inert matter remain undissolved.
 Menstruum: solvent used for extraction.
 Marc: the insoluble material that remains extraction.
 “
Continued….

 Methods of Extraction
1.Maceration
2.Percolation
3.Decoction
4.Digestion
5.Infusion

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Extraction with reflux

• A mixture of reactants and solvent is placed in a suitable

vessel, such as a round bottom flask. This vessel is connected
to a water-cooled Liebig or Vigreux condenser, which is
typically open to the atmosphere at the top.
• The reaction vessel is heated in order to boil the reaction
mixture; vapours produced from the mixture are condensed by
the condenser, and return to the vessel through gravity.
• The purpose is to thermally accelerate the reaction by
conducting it at an elevated, controlled temperature (i.e. the
solvent's boiling point) and ambient pressure.

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Extraction with agitation

 Agitation is the movement of one or more

components of a mixture to improve contact.
 Putting into motion by shaking or stirring, often
to achieve mixing.

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Counter current extraction

 A method of multiple liquid-liquid extractions is countercurrent extraction.

 It permits the separation of substances with different distribution coefficients (ratios).
 A clever design known as Craig apparatus is used for this purpose (Lyman
C. Craig, 1943).

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Criag apparatus
 Craig apparatus consists of a series of glass tubes (r: 0, 1, 2..) that are designed and arranged such that the lighter liquid phase
is transferred from one tube to the next.
 The liquid-liquid extractions are taking place simultaneously in all tubes of the apparatus which is usually driven
electromechanically.
 The lower (heavier) phase of the two-phase solvent system (e.g. water, blue layer in the picture) is the "stationary phase" red
laver in the picture) is the "mobile phase", whereas the upper (lighter) phase (e.g. hexane , red layer in picture)
 Here, wet raw material is pulverized using toothed disc disintegrators to produce fine slurry.
 The material to be extracted is moved in one direction (generally in the form of fine slurry) within a cylindrical extractor
where it comes in contact with extraction solvent.
 Finally, sufficiently concentrated extract comes out at one end of the extractor while the marc falls out from the other end.

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FILTRATION
Filtration is a process of separation of solids from a fluid by passing the same through a porous medium that retains the
solids but allows the fluid to pass through.
THEORY:
 The mathematical models for flow through a porous medium, cake filtration, and granular bed filtration may differ,
but all follow this basic rule. The energy lost in filtration is proportional to the rate of tow per unit area.
 The flow of liquid through a filter follows the basic rules that govern flow of any liquid through a medium offering
resistance.
 The rate of flow may be expressed as:
Rate: Driving force/ Resistance

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Pressure filtration
 This process is owing to the difficulty in removing the cake they are mechanically complex
and expensive.
 The filtration rate is influenced by properties of the slury.
 The rate goes up with increased pressure.

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Plate and Frame Press

 Simplest of all pressure filters.

 Most widely used press.
 Used for a high degree of clarification of the fluid.
 When clarity is the main objective, a "batch" mode
of operation is applied.
 As the name implies, the plate and frame filter press
is an assembly of hollow frames and solid plates
that support filter media.

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Advantages Disadvantages

 High solids content cake.  Large quantities of inorganic conditioning chemicals

are commonly used.
 Can dewater hard-to-dewater sludges.
 High capital cost, especially for variable-volume filter
 Very high solids capture.
presses.
 Only mechanical device capable of producing a cake
 Replacement of the media is time consuming.
dry enough to meet landfill requirements in some
locations..

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Vacuum Filtration
 Employed on a large scale.
 Rarely used for the collection of crystalline precipitates or sterile filtration.
 Simple and reliable machines, and therefore have gained wide acceptance in
the chemical, food and pharmaceutical industries.

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Rotary Drum Filter
 This is divided into sections, each connected to a
discharge head..
 Each filter unit is rectangular in shape.
 Each unit has a perforated metal surface and is
covered with filter cloth.

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Advantages Disadvantages

 Developed to overcome large problem of filter press  It can not be used for mixture of colloidal and course
and leaf filter. It is very versatile filter. particles.
 It is used generally for those operation in which the  It must be used continuously.
volume is very large.
 It is used where colloidal particles.
 It is used for production of wallboard from gypsum.

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Centrifugal Filtration

 General class of solids recovery devices.

 Centrifugal force is used to affect the passage of the liquid
through the filter medium.
 This type of filtration is particularly advantageous when
very fine particles are involved.

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Perforated Basket

 The device consists of a perforated metal

basket mounted on a vertical axis.
 Rotation speed 20 to 25
revolutions per second.

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Advantages Disadvantages

 Centrifuges have a clean appearance and have little to no  The machine can be very noisy and can cause
odor problems. vibration.
 Not only is the device easy to install and fast at starting  The device has a high-energy consumption due to
up and shutting down, but also only requires a small area highG-forces.
for operation.
 High initial capital costs.
 They can be selected for different applications.
 The device is simple to operate.
 Centrifuge has more process flexibility and higher
levels of performance.

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Azeotropic Distillation

 The technique of addition of another component to form a new low boiling point azeotropic solution
such as benzene can be added to the solution of ethanol and water in azeotropic distillation.
 The azeotropic distillation unit consists of a container to feed the azeotrope, decanter and steamer.
 For example; the mixture of acetic acid and water can be separate out with the addition of an ester
like n-butyl acetate.
 Remember the boiling point of acetic acid is 118.1°C and water is100°C.
 Addition of ester whose boiling point is 125°C forms a minimum-boiling azeotrope with water with
boiling point 90.2°C.

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Continued…..
 Hence azeotropic mixture will be distilled over as
vapor and leave acetic acid at bottoms. The
overhead vapor is condensed and collected in a
decanter.
 Here it forms two insoluble layers in which the top
laver contains pure butyl acetate with water, and a
bottom layer contains pure water saturated with
butyl acetate.
 The top layer is returned to the distillation column
and bottom layer is sent to another column for the
recovery of the ester by steam stripping.

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How it works.
 The entrainer decreases the boiling point of azeotropic solution and separates the components of mixture at
different boiling points.
 When azeotropic mixture is heated with entrainer, the condensed over head vapor forms two liquid phases
and collects in the decanter.
 In decanter, the top layer contains benzene whereas bottom layer contains water.
 The top layer of benzene again back to first column as reflux and source of entrainer whereas bottom layer
of water back to 2nd column.
 The bottom of 2nd column contains mixture of ethanol and water which transfers to 3rd column for
distillation.
 Third column contains pure water at bottom and distillate is returned to the1st column for recycling.

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Azeotropic distillation of ethanol

 Another example of azeotropic distillation is separation of ethanol with water from its aqueous solution.
 The boiling point of water is 100 °C and boiling point of ethanol is 78.3°C.
 By addition of benzene to the azeotropic mixture as entrainer, ethanol can be separated out from the solution.
 Presence of benzene forms a new solution of minimum boiling point with 22.8 mole% ethanol, 23.3 mole% water
and 53.9 mole% benzene which boils at 64.86 °C.
 Pure water leaves as the overhead product and pure ethanol leaves the column as bottoms product.

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Steam Distillation

 Is a special type of distillation (a separation process)for

temperature sensitive materials like natural aromatic compounds.
 It once was a popular laboratory method for purification of
organic compounds, but has become obsolete by vacuum
distillation.
 Steam distillation remains important in certain industrial sectors.

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Continuied…
 Many organic compounds tend to decompose at high sustained temperatures.
 Separation by distillation at the normal (1 atmosphere boiling points is not an option, so water or steam is introduced into
the distillation apparatus.
 The water vapor carries small amounts of the vaporized compounds to the condensation flask, where the condensed liquid
phase separates, allowing for easy collection.
 This process effectively allows for distillation at lower temperatures, reducingthe deterioration of the desired products.
 If the substances to be distilled are very sensitive to heat, steam distillation may be applied under reduced pressure,
thereby reducing the operating temperature further.
 After distillation the vapors are condensed.
 Usually the immediate product is a two-phase system of water and the organic distillate, allowing for separation of the
components by decantation, partitioning or other suitable method.

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Principle
 When a mixture of two practically immiscible liquids is heated while being agitated to expose the surface of each liquid
to the vapor phase, each constituent independently exerts its own vapor pressure as a function of temperature as if the
other constituent were not present.
 Consequently, the vapour pressure of the whole system increases.
 Boiling begins when the sum of the vapour pressures of the two immiscible liquids just exceeds the atmospheric
pressure (approximately 101 kPa at sea level).
 In this way, many organic compounds insoluble in water can be purified at a temperature well below the point at which
decomposition occurs.
 For example, the boiling point of bromobenzene is 156 °C and the boiling point of water is 100 °C, but a mixture of the
two boils at 95 °C.
 Thus, bromobenzene can be easily distilled at a temperature 61 °C below its normal boiling point.

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