CHAPTER 2

CONTINUOUS DISTILLATION COLUMN

2.1 SIZING AND CONFIGURATION DESIGN

2.1.1 SELECTION OF EQUIPMENT TYPE AND JUSTIFICATION

The removal of cyclohexane from the mixture of the cyclohexanol,

cyclohexanone, caproic acid and valeric acid is essential for the usage
unreacted cyclohexane to be fed back to the reactor. The separation of this
mixture is a liquid – liquid separation as all the components are in liquid
phase. The feed temperature of the mixture is to be 70 ˚C as it leaves the
cooler. Below are the basic details of the components for the consideration of
the equipment type.

Table 2.1: Basic details on the components of the mixture.

Boiling Melting
Molecular Density
Component Point Point Formula
Weight (kg/m3)
(°C) (°C)
Cyclohexane 80.74 6.55 C6H12 84.16 779
Cyclohexanol 160.8 25.93 C6H12O 100.158 962
Cyclohexanone 155.6 -16.4 C6H10O 98.15 948
Caproic Acid 205 -3.4 C6H12O2 116.1583 1000
Valeric Acid 187 -34.5 C5H10O2 102.13 1429
 Table 2.2: Comparison of Unit Operations for Cyclohexane Removal

Distillation Column Decanter Evaporator

Distillation is a Decanters are

The theory of
commonly used used to separate separation
unit operation for liquids where there mechanism of
the separation is a sufficient
evaporator is similar
process in the difference in
with distillation
industry. It involves density column by benefiting
the separation of a between the
from the different
mixture based on liquids for the
boiling points of
the difference in the droplets to settle component. The
Mechanism boiling point or readily. evaporation
volatility of its processes usually
components. and condensation from
separate
its volatility.
a single
Separation is be
component (typically
water) from a non-
volatile material. It
can be operated as a
single unit or multiple
units for heat re-
utilisation purposes.
Distillate Product: Light Product: Top Product:
Cyclohexane Cyclohexane Cyclohexane

Separation Bottom Product: Heavy Product: Bottom Product:

Product Cyclohexanol, Cyclohexanol, Cyclohexanol,
Cyclohexanone, Cyclohexanone, Cyclohexanone,
Valeric acid, Valeric acid, Valeric acid, Caproic
Caproic Acid Caproic Acid Acid
Basic figure of
equipment

Figure 2.1: Basic Figure 2.2: Basic Figure 2.3: Basic

Distillation Column Horizontal Decanter Evaporator Column

- A relative small - Required no - Suitable for

loss of energy input continuous process.
cyclohexane.
- Relatively cheaper
Advantages - Require less energy
- Higher purity of for operation.
cyclohexane for
recycling back to
the feed.
- Very high - Longer residence - Several units
energy input time up to 12 required to reach high
required hours purity of product which
will ultimately
- Very high - Slightly resemble a distillation
Disadvantages operational cost higher loss of column
cyclohexane
as compared - Low purity of
to distillation product.
process
- Slow process
 The cyclohexane that needs to be removed should have high
purity. This is to ensure that the continual of the oxidation of

Specification cyclohexane in the reactor to achieve same conversion. The

Required for residence time for the removal process should be as short as
Process possible to get a continuous flow of cyclohexane. The subsequent
mixture that is entering the second distillation column should least
cyclohexane, to ensure the purification of product to be efficient.

A distillation column is selected as a high purity of

cyclohexane can be obtained from the top flow. A high purity
Conclusion of cyclohexane obtained is essential for the efficient reaction
of subsequent reactor column and to avoid contamination of
subsequent column.
Table 2.3: Comparison on Type of Distillation Column for Cyclohexane Removal

Simple Distillation Extractive Azeotropic

Column Distillation Distillation Column
Column

The separation of Extractive The mixture that are

liquid mixtures by distillation also highly in nonideal
distillation involves the systems,with
depends on addition of the components having
differences in third component close boiling points
volatility between to the mixture among them, often
the components. which can be a produce azeotropes.
The greater the solvent or Azeotropes limit the
relative volatilities, entrainer. separation that can
Mechanism
the easier the be achieved by
separation. and condensationconventional
from its volatility. Separation is
distillation. In
azeotropic
distillation, the
equilibrium
behaviour of the
mixture is modiRed
by adding a new
material called the
solvent or entrainer.
 -
Effective - Effective for the - Ideal for the
separation for separation of separation of mixture
mixture that have close-boiling that contaion
different boiling point,pinched or azeotropic
points. azeotropic components.
- Do not need to systems. -- The added
add any solvent or - entrainer forms a
entrainers. - The use of minimum boiling
- Purity of the extractive point azeotrope with
product is equally distillation to one or more
Advantages high as the other obtain products components and
distillation. which residue distils overhead. The
- - Able to handle curve saddles are distillate is generally
high liquid flow made possible. heterogeneous, that
rates cost is, it is composed of
effectively. - two immiscible
- liquids when
condensed. Such a
heterogeneous
nature facilitates the
separation of the
product from the
entrainer.
- - Foaming can - Adding cost to Adding cost to
occur due to include solvent for include solvent for
agitation of the extractive extractive distillation
liquid by the vapor distillation of the of the mixture.
Disadvantages flowing up through mixture.
it. - The complexity of
- the operation is
- higher compared to
extractive and
normal distillation.
-
The mixture contains components of different boiling points.
Nature of Feed
There component that acquire to be removed do not form
azeotropes.
 The best method of distillation will be the multicomponent
continuous distillation that is sufficient enough for the removal

Conclusion of the cyclohexane. This method is economically also very

cost effective as the nature of feed to the column does not
need addition of any solvent for better separation. The purity
of the top product obtained can have high-quality.
Table 2.4: Comparison on Type of Internal Arrangement for Distillation Column
Packed Distillation
Column
The feed passes through
packing to maximize vapor-
liquid surface contact for an
efficient separation. Types of
Mechanism packing include dumped, or
random, packing and stacked
packing.
Basic Figure of
Column
Figure 2.4: Packed Bed
Column
Tray Distillation Column
The feed passes across the
plate/ tray that gives the vapor-
liquid interaction for the
separation.
The geometry of the trays within
the column affects the extent
and type of contact between the
vapor and liquid streams. Tray
types include sieve, valve, and
bubble cap.
Figure 2.5: Plate Column
 Most cost-efficient distillation Most cost efficient distillation
column when the diameter of column for diameters greater
the column is less than 0.6 m. than 0.6 m.

Because packing can be made The liquid/vapor contact in the

from inert materials, packed cross-flow of plate columns is
beds are able to handle more effective than the
corrosive materials. countercurrent-flow in packed
Advantages columns.
Lower pressure drop than in
plate columns preventing Cooling coils can easily be added
column flooding. to the plate column (cryogenic
applications).
Good for thermally sensitive
liquids. Can handle high liquid flow rates
cost-effectively.
Suitable for low pressure
operations.

Packing can break during Higher pressure drops than

installation, or due to thermal packed columns which could
expansion. cause column flooding.

Disadvantages Not cost efficient for high liquid Foaming can occur due to
flow rates. agitation of the liquid by the
vapor flowing up through it.
Contact efficiencies are
decreased when the liquid flow
rate is too low.

The tray distillation column is selected for the removal of

Conclusion cyclohexane as the flowrate of the feed is higher and the
efficiency of the distillation column is better for diameters greater
than 0.6m.
 Table 2.5: Comparison on Type of Tray for Distillation Column

Sieve Valve
Bubble Cap

The sieve tray are Valve Tray is using A bubble cap tray is
perforated trays with valve which is rise as perforated flat which
holes punched into vapor rate increase has a riser (chimney)
the plate. and then reduce as for each hole cover
Vapor comes out vapor rate fails, this with a cap
from the holes to stop the liquid from mounted.Usually
Mechanism give a multi orifice weeping. Valve can equipped with slots
effect. The vapor be round or to allow the passage
velocity keeps the rectangular, with or of vapor then the
liquid from flowing without caging vapor will contact
down through the structured. with liquid forming
holes. bubble on the next
tray.

Basic Figure
of Tray Type
Figure 2.6: Sieve Figure 2.7: Valve tray Figure 2.8: Bubble
tray Cap Tray
 Sieve tray has a Valve tray has It is able to operate
minimum capacity minimum capacity at
approximately 70%. approximately 60%. low vapor and liquid
rates.
Sieve tray is the Pressure drop is
cheapest comparing lesser than bubble Pressure drop is the
to bubble cap and cap but higher than highest among the
valve tray. sieve tray. three.
Advantages
Sieve trays give the Valve trays are
lowest pressure intended to give
drop. greater flexibility than
sieve trays at a lower
Sieve trays are the cost.
easiest to clean.

Bubble-caps are
Cannot operate at Cleaning is not as appreciably more
very low vapour easy as sieve tray. expensive than sieve
Disadvantages rates. or valve trays.

Most susceptible to
plugging.

Sieve trays are the cheapest and are satisfactory for the
Conclusion applications. It has a higher minimum capacity, ease of cleaning
and cost effective.