PRACTICAL GUIDE

Faculty Engineering and Technology

Department Chemical and Metallurgical Engineering

Chemical Engineering Laboratory 2

Course
(EHCEL2A)

Title Continuous Distillation

Compiled By S. Muthubi; N. Nyembe

Year Semester 1 - 2023

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GRADUATE ATTRIBUTE (GA)
Graduate attributes form a set of individually assessable outcomes that are components indicative
of the graduate’s potential to acquire competence to practice at the appropriate level. The
graduate attributes are exemplars of the attributes expected of graduates from an accredited
programme.

Experimentation and practical investigations are essential in the development of a graduate in

the engineering field. As such, the learner will be assessed in their ability to conduct
investigations of well-defined problems through locating and searching relevant codes and
catalogues, conduct standard tests, experiments and measurements. Therefore, the learner needs
to follow the competency indicators to be deemed competent in a GA. Competency indicators
are standard criteria the learner must use to achieve competency in a particular GA. For GA 5,
the competency indicators that need to be realized are as follows:

• Scope of the investigation is defined

• Investigations are planned and conducted within an appropriate practical
• Available literature is searched, and material is evaluated for suitability to the
investigation
• Relevant equipment is selected and appropriately used for the investigation
• Data obtained is analyzed and interpreted
• Conclusions are drawn from an analysis of all available evidence
• Purpose, process and outcomes of the investigation are recorded in a technical report

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1. INTRODUCTION
1.1. Main objective
The main objective of the practical is to separate a liquid mixture into its various components
using a distillation unit.

1.2. Specific objectives are:

• To conduct an energy and material balance around the column.

• To determine the number of theoretical plates using the McCabe-Thiele method.

• To determine the feed location stage.

2. THEORY
Distillation is a separation process, separating components in a mixture by making use of the fact
that some components vaporize more readily than others. When vapors are produced from a
mixture, they contain the components of the original mixture, but in proportions which are
determined by the relative volatilities of these components. The vapor is richer in some
components, those that are more volatile, and so a separation occurs.

The multi-stage distillation is a basic unitary operation of chemical industry. The liquid-vapor
separation (L-V) is a process which has been used for many years. There are many methods and
devices that have been developed to obtain the balance between the phases in contact.

The mass transfer increase in proportion with the contact area between the phase and this is the
reason why the device has 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%.

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.

2.1. Hypothesis 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

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2.2. Enriching section
Overall balance

V= L + D (1)

Balance on volatile component

V*yN+1 = L*xn + D*xd (2)

Can be represented as:

V*y = L * x + D * xd (3)

That is:

y = L/V * x + D/V * xd (4)

substituting equation (1) in the equation (4) and dividing by D and with reflux ratio defined by:

L/D = r (5)

The result is:

y = r/(r+1).x + xd/(r+1) (6)

2.3. Stripping section

L’ = V’ + R (7)

And the balance of the volatile component:

L’.xN’+1 = V’.yN’ + R.xR (8)

If the indices are omitted, this equation becomes:

y = L’/V’.x – R/V’.xR (9)

This is the Operating line of the stripping column intersecting the point:

R= (yR= xR, xR)

NB: the operating line of the stripping column can only be plotted if the flow rates L’ and V’ are
known.

However, if these data are not known, the operating line of the stripping column can be drawn
through the method of the feed line and the known degree of vaporization

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3. METHODOLOGY
3.1. Description of equipment
• 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. Consumables required

• Methanol
• Distilled water

3.3. Additional equipment

• One liter measuring cylinder
• Weighing balance
• Glass beakers

3.4. Utilities required

• Power supply: three-phase, P=3.5 kW
• Tap water for cooling
• Compressed air

3.5. Experimental procedure

A 15 L methanol/water mixture is to be synthesized and the mixture is to contain methanol at
a concentration of 30% (w/w).

3.5.1. Start Up
• Set all switches to 0
• Check that the emergency pushbutton is not pressed
• Connect the plant to the electrical mains
• Shut off valves V2, V3, V4, V5, V7, V8, V9, V10, V11, V12, V14, V21, V23 and V26
• Open valves V1, V15, V16, V17, V18, V19, V22 and V27
• Valve V6 is permanently opened to avoid overpressure in the feeding line
• Open partially valve V25
• Fill the boiler with the mixture to be distilled until the electrical resistor J2 is completely
plunged
• Fill the tank D1 with the mixture to be distilled
• Turn the switch AUTO-PC to AUT
• Connect the E.L.C.B switch
• Push the “Start” button

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 • Set the switch of resistor J2 to 1
• Power the electrical resistor using the output 4-20 mA of the 2nd loop of the controller
no.2, proportional to 0-2500 W (select the 2nd loop with pushbutton Loop and then the
indication Out with pushbutton Ind, finally increase its value with pushbutton to
▲100%).
• Connect the plant to the tap water using the rubber hose
• Wait for the solution to boil
• Take the mixture to the boiling point and then decrease the heating power 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%).
• Open the tap water
• Let the column to total reflux for about 5 minutes (until the temperature TI6 is stable)
• Turn the switch of the pump G1 to position 1.
• Feed, e.g. 5L/h (about 40%), using the output of the 4th loop of controller no. 1 (select
the 4th 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
• Select the 1st loop (TIC1) of controller no.1
• Select loop with pushbutton Loop and then the indication Out with pushbutton Ind,
finally increase or decrease its value with pushbutton ▼ ▼to e.g. 50%
• Switch on the heater J1
• Open valve V4
• The preheating temperature must be less than the boiling point of the mixture
• To select the reflux ratio, turn the switch for reflux to position 1
• Select the Start and Stop times (sec) on the timers, to give the desired reflux ratio
• Open valve V13 partially
• Run the column for 20 minutes
• Measure the flow rate of cooling water

3.5.2. Shut Down

• Set the “Reflux” switch to 0
• Set the switch of resistor J1 to 0
• Set the switch of pump G1 to 0
• Close valve V1
• Set the switch of the heating resistor J2 to 0
• Close valve V13
• Drain tank D2, D3 and D4
• Close the tap water
• Disconnect the E.L.C.B
• Switch off the plant from the power supply

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4. DATA COLLECTION

Table 1: Observation sheet

Products (20 minutes)

Distillate Bottoms
product product
Temperature
(°C)
Mass (g)
Volume (mL)

5. CALCULATIONS
• Calculate XB and XD
• Determine the number of theoretical stages
• Perform energy balance

6. PHYSICAL PROPERTIES
Below are empirical equations that must be used to determine the physical properties required
for the calculations.

Density equation:

Substance C1 C2 C3 C4
Water 5.459 0.30542 647.13 0.081
Methanol 2.288 0.2685 512.64 0.2453

C1
𝜌= T ; (kmol/m3) where T is temperature in Kelvins
(1+(1− )C4 )
C2 C3

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Molecular weight:

Atomic weight (g/mol)

Substance
C H O
Water (H2O)
12.0107 1.0079 16
Methanol (CH3OH)

Heat of vaporization equation:

Tc
Substance C1 C2 C3 C4
(K)
Water 5.2053×10+07 0.3199 -0.212 0.25795 647.13
Methanol 5.2390×10+07 0.3682 0 0 512.64

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∆𝐻𝑣 = 𝐶1 × (1 − 𝑇𝑟 )[𝐶2+(𝐶3×𝑇𝑟 )+(𝐶4×𝑇𝑟 )] ; (J/kmol)
where Tr = 𝑇⁄𝑇 is temperature in Kelvins
𝑐
Tr is the reduced temperature.
Tc is the critical temperature.

Heat capacity equation:

Substance C1 C2 C3 C4 C5
Water 2.7637×10+05 -2.0901×10+03 8.1250×10+00 -1.4116×10-02 9.3701×10-06
Methanol 1.0580×10+05 -3.6223×10+02 9.3790×10-01 0 0

𝐶𝑝 = 𝐶1 + (𝐶2 × 𝑇) + (𝐶3 × 𝑇 2 ) + (𝐶4 × 𝑇 3 ) + (𝐶5 × 𝑇 4 ) ; (J/kmol.K)

where T is temperature in Kelvins

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7. EQUILIBRIUM DATA

Methanol Liquid Mole Methanol Vapor Mole

Fraction Fraction
0 0
0.067 0.330
0.133 0.493
0.200 0.589
0.267 0.654
0.333 0.702
0.400 0.741
0.467 0.775
0.533 0.805
0.600 0.833
0.667 0.861
0.733 0.888
0.800 0.915
0.867 0.942
0.933 0.971
1 1