1 INTRODUCTION

1.1 Background
Distillation is the separation of liquid or vapor mixtures into their various components is one and
also the most widely used method. In processing, the demand for purer products, coupled with
the need for greater efficiency, has promoted continued research into the techniques of
distillation. A distillation unit should be considered together with its associated control system,
and it is often operated in association with several other separate units. In this context, the basic
problems of design are considered and it may be seen that not only the physical and chemical
properties, but also the fluid dynamics inside the unit, determine the number of stages required
and the overall layout of the unit (Richardson, 2002).

1.2 Main objective

The main objective of this practical is to understand the construction, design and operational
characteristics of a continuous distillation system.

1.3 Specific objectives are:

 To perform energy and material balance around the column
 To determine the effect of reflux ratio on the composition of the distillate
 To determine the number of theoretical plates using McCabe-Thiele and Lewis-Sorel method
and compare the results.
 Feed: 15L of mixture at 28% weight of methanol.
 Operate for 1 hour at reflux ratio 1:1, 1:2 or 2:1

1.4 Scope
A pilot plant will be used to perform the distillation process as there will be a continuous
addition of water to the plant. Various calculations will be made to perform a material balance
and to determine the effect of the reflux ratio on the compositions, there are two methods which
will be used and those methods will also lead to finding the theoretical stages and how the results
differ has to be figured out.

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2 LITERATURE REVIEW

2.1 What is Distillation?

A process in which a liquid or vapour mixture of two or more substances is separated into its component
fractions of desired purity, by the application and removal of heat. Distillation is the most common
separation technique, it consumes enormous amounts of energy, both in terms of cooling and heating
requirements and can contribute to more than 50% of plant operating costs (Leswifi, 2017).

Consider a two component mixture: a simple binary system of 50% water and 50% methanol: Pure
water has a boiling point of 100 degrees and pure methanol has a boiling point of 65 degrees. But the
50-50 mixture of methanol and water has a boiling point of 84 degrees. At the mixture boiling point of
84 degrees Celsius pure methanol has a vapour pressure of 200 kPa and pure water has a vapour
pressure of 60kPa. Based on these physical properties, we say that methanol is the MORE VOLATILE
COMPONENT, because it has the lower boiling point OR because it has a higher vapour pressure, and
water is the LESS VOLATILE COMPONENT, because it has a higher boiling point OR because it has a lower
vapour pressure (Leswifi, 2017).

2.2 The principle of Continuous Distillation

The separation process is usually carried out in columns which consist of devices enabling the
continuous or discontinuous liquid-vapor contact. The plate columns are the example of discontinuous
balance states, while the filling columns are example of continuous liquid-vapor contact (SGF
Mncwango, 2017).

The mass transfer increase in proportion with the contact area between the phase and this is the reason
why the device have been planned to obtain the maximum interface area. With constant liquid and
vapor flows, the contact time between the two phases is constant so when the contact area increase, so
does the mass transfer and with it the possibility to reach the balance of the system, which represent
the 100% of efficiency. However, the combination of factors such as the production of contact devices,
the operative conditions and the characteristics of the system rarely take it to an efficiency of 100% (SGF
Mncwango, 2017).

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2.2.1 Hypotheses of ideal conditions:
• Each stage of the column corresponds to an ideal stage of the process: the liquid and vapor leaving
each stage are in thermodynamic equilibrium.

• The column is adiabatic (there is no heat exchange with the outside)

• Reflux occurs at the boiling point.

• The molar flow rates of liquid and vapor are constant along the column.

• Molar specific heat and molar heat of vaporization do not depend on the composition (SGF
Mncwango, 2017).

2.3 Analysis of distillation in tray towers: McCabeThiele Method

McCabe and Thiele (1925) developed a graphical method to determine the theoretical number of
stages required to effect the separation of a binary mixture (McCabe and Smith, 1976). This method
uses the equilibrium curve diagram to determine the number of theoretical stages (trays) required to
achieve a desired degree of separation. It assumes constant molar overflow and this implies that: (i)
molar heats of vaporization of the components are roughly the same; (ii) heat effects are
negligible. The information required for the systematic calculation are the VLE data, feed condition
(temperature, composition), distillate and bottom compositions; and the reflux ratio, which is
defined as the ratio of reflux liquid over the distillate product.

The feed has a concentration of xF

(mole fraction) of the more volatile

component, and a distillate having a concentration of x

of the more volatile

component and a bottoms having a concentration of x

is desired. In its essence,

the method involves the plotting on the equilibrium diagram three straight lines:

the rectifying section operating line (ROL), the feed line (also known as the q line) and the
stripping section operating line (SOL). An important parameter in

the analysis of continuous distillation is the Reflux Ratio, defined as the quantity

of liquid returned to the distillation column over the quantity of liquid withdrawn as

product from the column, i.e. R = L / D. The reflux ratio R is important because

the concentration of the more volatile component in the distillate (in mole fraction

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x

) can be changed by changing the value of R. The steps to be followed to

determine the number of theoretical stages by McCabe-Thiele Method:

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3 METHODOLOGY

3.1 Equipment Description

 The continuous distillation plant is mainly composed of a mash-packing column, bottom
boiler with electrical heater, a condenser and a feed pump.
 The binary mixture, stocked in tank is fed with a column feed pump after it has
been preheated by an electrical heater.
 Once the boiler has been filled, the solution is heated with the bottom resistor.
 Once the solution reaches the boiling point and the column is in steady state the distillate
can be taken, keeping reflux ratio as fixed, and then it can be fed.
3.2 MATERIALS AND CHEMICALS
3.2.1 Consumables Required
 Methanol
 Distilled Water

3.2.2 Utilities Required

 Power supply: three phases. P= 3.5kW
 Tap water max: 300l/h at 2 bars
 Compressed air.

3.3 Experimental Procedure

For Start-up process, all switches will be set to 0 and also checking that the emergency
pushbutton is off. The column will be operated for an hour with the desired reflux ratios. The
plant will be connected to the electrical mains for some time. Valves V2, V3, V4, V5, V7, V8,
V9, V10, V11, V12, V14, V21, V23 and V26 will be closed while valves V1, V15, V16, V17,
V18, V19, V20, V22 and V27 will be opened. Valve V6 will be permanently opened to avoid
overpressure in the feeding line. V25 will be partially opened and the boiler filled with the
mixture to be distilled until the electrical resister is completely plunged.

The tank D1 will be filled with the mixture that is to be distilled, while the AUTO-PC switch
will be turned to AUT. The E.L.C.B switch will be connected and the start button pushed. The
switch of the resister J1 will be switched to 1. The electrical resistor will be powered using the
output 4-20mA of the 2nd loop of the controller no.2, proportional to 0-2500W (select the 2 nd loop

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with pushbutton loop and then the indication Out with pushbutton Ind, finally increase its value
with pushbutton to ▲ 100%). The plant will then be connected to the tap using a rubber hose.

The mixture will be heated to the boiling point, upon reaching boiling point the heating power
will be decreased to 60% (select the 2nd loop with pushbutton loop and then the indication Out
with pushbutton Ind, finally decrease its value with pushbutton ▼ to 60%) as Valve V13 will be
partially opened. The column is left at total reflux for about 5 minutes (until the temperature Ti6
is stable), the switch of the pump G1 will be turned to position 1 while 5l/h (about 40%) is fed
using the output of the 4th loop of controller no.1 (select the 4 th (G1) loop with pushbutton loop
and then the indication Out with pushbutton Ind, finally increase or decrease its value with
pushbutton ▼ ▲ to e.g.40%). Wait until the container of the preheating resistor J1 is filled. The
1st loop (TIC1) of controller no.1 will be then selected and the set point adjusted (push the button
SP-w increase or decrease its value with pushbutton ▲ ▼) to 50°C. Heater J1 will be switched
on until the preheating temperature is less than the boiling point of the mixture. In order to select
the reflux ratio, the different times will be selected on the timers. The temperatures along the
column will give the composition in different positions of the column.

For the shut-down process, the switch of resistor J1 will be set to 0 and pump G1 stopped. The
switch of the heating resistor J2 will also be set to 0 and that of the Reflux will be set to 0. V13
and the tap water will be closed while tanks D2, D3 and D4 will be drained. The E.L.C.B will be
disconnected and the plant will be switched off from the power supply.