BATANGAS STATE UNIVERSITY

College of Engineering, Architecture & Fine Arts

Gov. Pablo Borbon Campus II, Alangilan, Batangas City, Philippines 4200
www.batstate-u.edu.ph Telefax: (043) 300-4404 locs. 106-118

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

FE 523
Materials Handling and Separation Process

DISTILLATION

Group 1
Abdon, Rena Faith
Adia, Kenneth E.
Alegria, Christine Mae
Aprid, John Aldousch
Bagon, Shaina

Engr. Nico John R. Abratique

Instructor

August 20, 2018

HISTORY

As far back as the fourth century B.C. Aristotle suggested the possibility of spirit distillation
when he wrote: "Seawater can be made potable by distillation as well and wine and other liquids
can be submitted to the same process." It is an age-old process which may have begun as early as
2000 BC.
Some say that the first use of distillation occurred in China, Egypt, or Mesopotamia for
medicinal purposes as well as to create balms, essences, and perfumes. About 1810 B.C. in
Mesopotamia, the perfume of King Zimrilim employed this method to make hundreds of liters of
balms, essences and incense from cedar, cypress, ginger and myrth every month. These were used
to embalm the dead and for spiritual, medicinal and cosmetic purposes (Unguentarium, 2018).
Clear evidence of the distillation of alcohol comes from the School of Salerno in the 12th
century. Fractional distillation was developed by Tadeo Alderotti in the 13th century.
In the early 19th century the basics of modern techniques including pre-heating and reflux
were developed, particularly by the French, then in 1830 a British Patent was issued to Aeneas
Coffey for a whiskey distillation column, which worked continuously and may be regarded as the
archetype of modern petrochemical units.

TRIVIA

It was a Persian doctaor, Avicenna (980-1037), who was the first to obtain the oil from
flowers, known as attar, by distillation. Before this revelation, perfumes were derived from the
bark of twigs and shrubs in the form of resins. His works were faithfully followed by other
chemists, soon becoming general practice.
The development of distillation by Avicenna made the production of essential oils and scented
waters such as rosewater possible. These were used for a wide variety of purposes, scenting rooms
and linen as well as toiletries.
Bourbon is the official distilled spirit of the United States
When first made, distilled spirits are completely clear with no color. They get their colors and
hues from the aging process in oak barrels.

USES

Distillation is a physical process that uses heat to purify or separate mixtures containing one or
more liquids. As a mixture is heated, the liquid with the lowest boiling point will boil and turn into
vapor, leaving behind any solid material or other liquids. The vapor is captured and cooled until it
condenses, resulting in a purified version of the liquid.
A plant that performs distillation is called a distillery. The apparatus used to perform
distillation is called a still.
Distillation is used for many commercial processes, such as the production of gasoline,
distilled water, xylene, alcohol, paraffin, kerosene, and many other liquids (Helmenstine, 2017).
Some uses of distillation:
 Salt water is turned into fresh water through distillation.
 Various forms of fuel, such as gasoline, are separated from crude oil by distillation.
 Gas may be liquefied and separate. Nitrogen, oxygen, and argon are distilled from air.
 Water from natural sources contains a variety of minerals and other impurities, many of
which can be removed by distillation.
 Desalination plants also use distillation to turn seawater into drinking water
 Distillation is used to produce a variety of alcoholic beverages, such as whiskey, rum and
brandy.
 The aroma from various plants and herbs is contained in what are known as essential oils,
which can be extracted through distillation.
 Steam distillation is also used to create natural food flavorings. The most common are
citrus oils and liquid extracts of various herbs and spices (Maxfield, 2018).

IMPORTANCE
Distillation is an important commercial process that is used in the purification of a large
variety of materials. Distillation is among the most important and widely used industrial
operations today. About 95 percent of all separation processes today are carried out in industry
with more than 40,000 distillation systems.
It is the primary method used for purifying drinking water on both a large and small scale.
There are many models available for purifying water on a smaller scale. Simple distillation is also
a primary method for the purification of ethanol into fuel grade alcohol. The alcohol industry uses
simple distillation to improve the concentration of alcohol.
Simple distillation technology can help improve water purity in underdeveloped countries, or
areas that have lost the use of municipal water systems. Simple water distillation helps remove
impurities and reduces waterborne illness by improving the water's quality.

TYPES OF DISTILLATION

1. DIFFERENTIAL DISTILLATION

Simple distillation, also known as Rayleigh distillation or differential distillation, is the

most elementary example of batch distillation. In this distillation system, the vapor is removed
from thestill during a particular time interval and is condensed in the condenser. The more
volatile component is richer in the vapor than in the liquid remaining in the still. Over time, the
liquid remaining in the still begins to experience a decline in the concentration of the more
volatile component, while the distillate collected in the condenser becomes progressively
more enriched in the more volatile component.
 No reflux is returned to the still, and no stages or packing materials are provided inside
the column; therefore, the various operating approaches are not applicable to this distillation
system.

2. FLASH DISTILLATION

Flash distillation (sometimes called "equilibrium distillation") is a single stage separation

technique. A liquid mixture feed is pumped through a heater to raise the temperature and
enthalpy of the mixture. It then flows through a valve and the pressure is reduced, causing the
liquid to partially vaporize. Once the mixture enters a big enough volume (the "flash drum"),
the liquid and vapor separate. Because the vapor and liquid are in such close contact up until
the "flash" occurs, the product liquid and vapor phases approach equilibrium.

3. FRACTIONAL DISTILLATION

Fractional distillation is the separation of a mixture into its component parts, or fractions,
such as in separating chemical compounds by their boiling point by heating them to a
temperature at which one or more fractions of the compound will vaporize. It is a special type
of distillation. Generally the component parts boil at less than 25 °C from each other under a
pressure of one atmosphere. If the difference in boiling points is greater than 25 °C, a simple
distillation is used.

4. BATCH DISTILLATION

Batch distillation refers to the use of distillation in batches, meaning that a mixture is
distilled to separate it into its component fractions before the distillation still is again charged
with more mixture and the process is repeated. This is in contrast with continuous distillation
where the feedstock is added and the distillate drawn off without interruption. Batch
distillation has always been an important part of the production of seasonal, or low capacity
and high-purity chemicals. It is a very frequent separation process in the pharmaceutical
industry.

5. ENHANCED DISTILLATION

Several enhanced distillation-based separation techniques have been developed for

close-boiling or low-relative-volatility systems, and for systems exhibiting
azeotropicbehaviour. These enhanced techniques can be classified according to their effect on
the relationship between the vapor and liquid compositions:

a) AZEOTROPIC DISTILLATION

This term has been applied to a broad class of fractional distillation-based

separation techniques when specific azeotropicbehaviour, often called the entrainer, may
already be present in the feed mixture (a self-entraining mixture) or may be an added mass
 separation agent. Azeotropic distillation techniques are used throughout the
petrochemical and chemical processing industries for the separation of close-boiling,
pinched, or azeotropic systems for which simple distillation is either too expensive or
impossible.

b) EXTRACTIVE DISTILLATION

Extractive distillation is a partial vaporization process in the presence of a miscible,

high-boiling, nonvolatile mass separation agent, normally called the solvent, which is
added to an azeotropic or nonazeotropic feed mixture to alter the volatilities of the key
components without the formation of any additional azeotropes. It can also be used to
obtain products which are residue curve saddles, a task not generally possible for
single-feed distillation.

c) REACTIVE DISTILLATION

It is a unit operation in which chemical reaction and distillation are carried out
simultaneously within a fractional distillation apparatus. Reactive distillation may be
advantageous for liquid-phase reaction systems when the reaction must be carried out
with a large excess of one or more of the reactants, when a reaction can be driven to
completion by removal of one or more of the products as they are formed, or when the
product recovery or by-product recycle scheme is complicated or made infeasible by
azeotrope formation.

BASIC DISTILLATION EQUIPMENT AND OPERATION

 MAIN COMPONENTS OF DISTILLATION (Columns)

 VERTICAL SHELL
- where the separation of liquid components is
carried out

 COLUMN INTERNALS
- such as trays/plates and/or packings which are used to enhance component separations

 REBOILER
- to provide the necessary vaporization for the distillation process
 CONDENSER
- to cool and condense the vapour leaving the top of the column

 REFLUX DRUM
- to hold the condensed vapour from the top of the column so that liquid (reflux) can be
recycled back to the column

 CONTINUOUS DISTILLATION
 DISTILLATION COLUMN
- This is the main equipment where the separation process described above is carried out.
In general, the distillation column is separated into 3 sections: rectifying (or enriching)
section, stripping (or exhausting) section and feed (or flashing) section. At the
rectifying section, the more volatile component is removed through contacting the
rising vapour with the down-flowing liquid. At the stripping section, the down-flowing
liquid is stripped of the more volatile component by the rising vapour.

 OVERHEAD CONDENSER
- This is a heat exchange equipment for condensing the hot vapour leaving the top of the
distillation column. Either cooling water (e.g. using shell-and-tube heat exchanger) or
air (using fin-fan condensers) can be used as the cooling medium. In either case, partial
or total condensation may be achieved.

 OVERHEAD ACCUMULATOR
- This is a horizontal (usually) pressure vessel whereby the condensed vapour is
collected.
 PUMPS
- Pumps can be used for returning the reflux liquid back to the distillation column, or for
pumping out the bottoms product for storage, or for pumping the feed into the
distillation column.

 REBOILER
- The purpose of the reboiler is to produce the vapour stream in the distillation column,
called the reboiled vapour or the boil-up vapour. Reboilers can be both external or
internal (stab-in). Steam reboilers or fired reboilers can be used. Fired reboilers
typically uses fuel gas or fuel oil or combination of both.
 FEED/BOTTOM EXCHANGER
- The heat exchanger is used for heat conservation: the hot bottoms stream is used to heat
up the feed stream before it enters the distillation column. As a result the bottoms
product is cooled and then rundown to storage. For better temperature control of the
feed stream, a separate preheater or charge heater (both not shown in the above
diagram) may be used. This is usually located downstream of the feed/bottom
exchanger for final temperature adjustment. Steam may be used for the preheater, and
fuel gas-fuel oil is used for the charge heater.

 CHARGE HEATER / STEAM PREHEATER

- This can be a fuel gas/fuel oil-fired heater or steam-heated exchanger for final
temperature control before the feed enters the column.
 PARTS
 LABORATORY DISTILLATION

The basic apparatus includes a retort stand. A ring support is clamped to the stand.
A round-bottomed flask sits on the ring support. This distilling flask contains a liquid that
is heated from underneath by a Bunsen burner. A thermometer sits in the neck of the flask
to allow monitoring of the vapor temperature. The thermometer allows the temperature of
the vapor to be controlled to correspond with the boiling point of the desired component in
the heated liquid.

 BASIC OPERATION AND TERMINOLOGY

o Feed – the liquid mixture that is to be processed and this is introduced usually
somewhere near the middle of the column to a tray known as the feed tray.
o Feed tray- divides the column into a top (enriching or rectification) section and a
bottom (stripping) section.
o The feed flows down the column where it is collected at the bottom in the reboiler.
Heat is supplied to the reboiler to generate vapour. The vapour raised in the reboiler
is re-introduced into the unit at the bottom of the column.
o The liquid removed from the reboiler is known as the bottoms product or simply,
bottoms. The vapour moves up the column, and as it exits the top of the unit, it is
cooled by a condenser. The condensed liquid is stored in a holding vessel known as
the reflux drum.
o Some of this liquid is recycled back to the top of the column and this is called the
reflux. The condensed liquid that is removed from the system is known as the
distillate or top product.
o Thus, there are internal flows of vapour and liquid within the column as well as
external flows of feeds and product streams, into and out of the column.
 COLUMN INTERNALS:
 BUBBLE CAP TRAYS
 - has riser or chimney fitted over each hole, and a cap that covers the riser. The cap is
mounted so that there is a space between riser and cap to allow the passage of vapour.
Vapour rises through the chimney and is directed downward by the cap, finally
discharging through slots in the cap, and finally bubbling through the liquid on the tray.

 VALVE TRAYS
- perforations are covered by liftable caps. Vapour flows lifts the caps, thus self-creating
a flow area for the passage of vapour. The lifting cap directs the vapour to flow
horizontally into the liquid, thus providing better mixing than is possible in sieve trays.

 SIEVE TRAYS
- are simply metal plates with holes in them. Vapour passes straight upward through the
liquid on the plate. The arrangement, number and size of the holes are design
parameters.

 TYPICAL STANDARD DESIGN

  PACKED BEDS

Standard Design of Distillation Packed Bed Distillation used in

Column (Packed Beds) Petrochemical Industry

Equipment Design
After the feed mixture enters the column liquid flows down the column through the
packing countercurrently and contacts the rising vapor stream. The liquid at the bottom enters a
reboiler. Two streams exit the reboiler; a vapor stream, which returns to the column, and a liquid
product stream. The vapor stream flows upward through the packing, picks up the more volatile
components, exits the column, and enters a condenser. After the vapor condenses, the stream
enters a reflux drum, where it is split into an overhead product stream, known as the distillate,
and a reflux stream that is recycled back to the column.

 PLATE / TRAY COLUMN

Standard Design of Distillation Plate Distillation Column used for

Column (Plate) mineral oils
Equipment Design
After the feed mixture enters the column, liquid flows down the column and across the
trays in either crossflow or countercurrent flow. A reboiler at the bottom separates the stream
into a vapor stream that returns to the column and a liquid product stream. The vapor stream
flows upward through the trays, and contacts the down-flowing liquid stream, allowing the
separation to take place. At the top of the column, the vapor is condensed in a condenser. The
condensed stream which is shown in blue, is split into an overhead product stream, known as the
distillate, and a reflux stream that returns to the top of the column.

CRITICAL FACTORS TO VAPOR LIQUID EQUILIBRIUM DURING

DISTILLATION

1. RELATIVE VOLATILITY
During distillation, substances separate based on their boiling points. The
boiling point of the mixture varies as vapor rises in a distillation column, due to
changes in temperature and pressure.

2. ACTIVITY COEFFICIENT-SURFACE TENSION

Surface tension must be considered because it can cause deviations in expected
behavior in a mixture of chemical substances. This is where activity coefficient
comes in.

3. SOLUBILITY
Solubility changes with temperature and pressure, which means it may become
harder to separate two substances as distillation progresses.

4. MAXIMUM ACHIEVABLE CONCENTRATION

There is always a limit to the concentration of a certain substance that is
achievable through distillation. Repeated distillation can refine a mixture only to the
maximum achievable concentration, after which point distillation cannot further
separate the substances.

5. SURFACE AREA
Achieving the optimum amount of surface area for the liquid and vapor present
in a distillation column maximizes the efficiency of a distillation column.