MODULE 2 (Institute of food Technologists – IFT)

(WEEK5-6)
For the unit operations and practical and emerging technologies, the principles and process should be
thoroughly described (NO COMPUTATION). The industries utilizing such operations, equipment involved,
and their products should be enumerated. Applications should also be described. Related diagrams,
figures, pictures, and videos SHOULD BE shown to class. References should be cited.

DISTILLATION

Principles

Distillation

- a very old technique dating back to the first century A.D

- highly developed in all respects, i.e. fundamentals (thermodynamics, vapor liquid equilibrium),
process design as well as equipment (packed columns, tray columns)
- the most important technique for separating fluid mixtures into pure substance in the process
industries (and consensus is that it will remain so for years to come)
- it carries out approximately 95% of all liquid separations
- its exceptional role is founded on the fact that distillation is the only separation technique that is
capable to fractionate a fluid mixture into its pure constituents
- its separation process is driven by difference in component volatilities

Disadvantages:

- risk of thermal degradation of the species (kaya often not used for biochemical processes)
- high energy demand

Principle of distillation

1. generation of a two-phase system

2. mass transfer across the interface
3. separation of the two phases

**in most alternative separation processes, e.g. absorption, adsorption, and extraction, the two phase
system is created by the addition of an external substance (entrainer or solvent) that has to be removed
later on in an additional separation process. In distillation however, the two phase system (vapor-liquid)
is generated by a supply of heat which can easily be removed later on.
Fundamentals

Basic principle: to bring a liquid into intimate contact with a vapor so that mass transfer between the
two coexistent phases takes place.

Interfacial mass transfer driving force: the endeavor of each system to reach a state of equilibrium.

(Therefore, a good knowledge of vapor liquid equilibrium is of essential importance for the design of
distillation processes.)

In distillation,

 the concentrations of the vapor ( y ) and the liquid ( x ) must be different.

 the liquid is at the boiling point and the vapor at the dew point.
 the region between the boiling and the dew points is used

(A liquid mixture approaches the boiling point either by rising the temperature or by decreasing the
pressure. Analogously, a vapor mixture reaches the dew point either by decreasing the temperature or
by increasing the pressure)

Industrial distillation is typically performed in distillation towers or distillation columns (D=65 cm-6 m,
H=6-60m).

When the process feed has a diverse composition, as in distilling crude oil, liquid outlets at intervals up
the column allow for the withdrawal of different fractions or products having different boiling points or
boiling ranges. The "lightest" products (those with the lowest boiling point) exit from the top of the
columns and the "heaviest" products (those with the highest boiling point) exit from the bottom of the
column and are often called the bottoms.

Reflux

- used to achieve a more complete separation of products

- the portion of the condensed overhead liquid product from a distillation or fractionation tower
that is returned to the upper part of the
- (Inside the tower, the downflowing reflux liquid) provides cooling and condensation of the
upflowing vapors, thereby increasing the efficacy of the distillation tower

The more reflux is provided for a given number of theoretical plates, the better is the tower's separation
of lower boiling materials from higher boiling materials. Alternatively, the more reflux is provided for a
given desired separation, the fewer theoretical plates are required.

Distillation columns (distillation towers) are made up of several components, each of which is used
either to transfer heat energy or enhance material transfer. A typical distillation column consists of
several major parts:

1. A vertical shell where separation of the components is carried out.

2. Column internals such as trays, or plates, or packings that are used to enhance component
separation.
 3. A reboiler to provide the necessary vaporization for the distillation process.
4. A condenser to cool and condense the vapor leaving the top of the column.
5. A reflux drum to hold the condensed vapor from the top of the column so that liquid (reflux) can
be recycled back to the column.

The vertical shell houses the column internals and together with the condenser and reboiler constitutes
a distillation column (Fig. 4.5).

Distillation can be used in various ways

1. continuous flash distillation

2. fractional distillation
3. batch distillation
4. steam distillation

Process

Batch distillation (Fig. 16) is often preferable to continuous distillation when small quantities of feed
material are processed. A liquid feed is charged to a still pot and heated until vaporization occurs. Vapor
leaves the top of the column, and after condensation, part is removed as product and the rest returned
to the column as reflux. As distillation proceeds, the contents of the still pot and the overhead product
become richer in less volatile components. When operated at a fixed reflux ratio, an overhead product
cut is collected until the product composition becomes unacceptable. As an alternative, the reflux ratio
can be gradually increased to hold the product composition constant as the cut is taken. For a fixed rate
of heat addition to the still pot, the latter option results in a steadily declining product flow rate. After
the first cut, subsequent cuts can be taken to obtain lower volatility products. Intermediate cuts of mixed
composition are sometimes taken between each product cut, and these are saved and later returned to
the still pot for inclusion in the next batch.

Heating an ideal mixture of two volatile substances A and B (with A having the higher volatility, or lower
boiling point) in a batch distillation setup (such as in an apparatus depicted in the opening figure) until
the mixture is boiling results in a vapor above the liquid which contains a mixture of A and B. The ratio
between A and B in the vapor will be different from the ratio in the liquid: the ratio in the liquid will be
determined by how the original mixture was prepared, while the ratio in the vapor will be enriched in
the more volatile compound, A (due to Raoult's Law, see above). The vapor goes through the condenser
and is removed from the system. This in turn means that the ratio of compounds in the remaining liquid
is now different from the initial ratio (i.e. more enriched in B than the starting liquid).

The result is that the ratio in the liquid mixture is changing, becoming richer in component B. This causes
the boiling point of the mixture to rise, which in turn results in a rise in the temperature in the vapor,
which results in a changing ratio of A : B in the gas phase (as distillation continues, there is an increasing
proportion of B in the gas phase). This results in a slowly changing ratio A : B in the distillate.
If the difference in vapor pressure between the two components A and B is large (generally expressed as
the difference in boiling points), the mixture in the beginning of the distillation is highly enriched in
component A, and when component A has distilled off, the boiling liquid is enriched in component B.

Fractional distillation produces more efficient separations than simple distillation. It can be performed in
a continuous mode involving continuous sample feed to the column or a batch mode where a discrete
batch of sample is placed in the boiling flask. Most laboratory fractional distillations are performed in
batch mode. In fractional distillation, part of the condensed vapour, the reflux, returns to the still,
meeting the rising vapour in its passage. This type of distillation is an equilibrium process in which the
composition of the boiling liquid and the distillate is constantly changing as the distillation proceeds. This
equilibrium is achieved by a countercurrent flow process occurring through contact of vapour and
condensed vapour at so-called plates or trays in a fractionating column. Hence, a fractionating column
and a reflux-ratio-controlling device are equipment requirements additional to those used for simple
distillation. The exchange of material and heat is a physical process taking place at the interface between
the two phases, and the surface area for exchange should therefore be as large as possible. This surface
can be provided by an empty column, but in most cases, surface area is increased by using columns
packed with spirals, helices, etc. or plate columns. Plate columns differ considerably in design although
the basic requirement is a series of practical plates fixed perpendicular to the axis of the column, thus
allowing the liquid and vapour phases to be mixed thoroughly. On the other hand, packed columns have
a number of advantages and are widely used in the laboratory. Their efficiency depends on the packing.

Continuous distillation is an ongoing distillation in which a liquid mixture is continuously (without

interruption) fed into the process and separated fractions are removed continuously as output streams
as time passes during the operation. Continuous distillation produces at least two output fractions,
including at least one volatile distillate fraction, which has boiled and been separately captured as a
vapor condensed to a liquid. There is always a bottoms (or residuum) fraction, which is the least volatile
residue that has not been separately captured as a condensed vapor.

Industries utilizing distillation, equipment involved, and their products (enumerate)

Industries utilizing distillation

 Petrochemical /Petroleum Refineries

 Distillation of crude oil
 Equipment involved:
 Products:
 Food
 Equipment involved:
 Products:

 Pharmaceutical
 Equipment involved:
 Products:
 Chemical
 Equipment involved:
  Products:
 Natural gas processing
 Equipment involved:
 Products:

Applications

separation of alcoholic liquors from fermented materials

separation of gasoline, kerosene, and lubricating oil from crude oil; separate crude oil into more fractions
for specific uses such as transport, power generation and heating

processing of such chemical products as formaldehyde and phenol

desalination of seawater

Air is distilled to separate its components - notably oxygen, nitrogen and argon - for industrial use.

Show related diagrams, figures, pictures, and videos

References